DR ANTHONY MELVIN CRASTO,WorldDrugTracker, helping millions, A 90 % paralysed man in action for you, I am suffering from transverse mylitis and bound to a wheel chair, With death on the horizon, nothing will not stop me except God................DR ANTHONY MELVIN CRASTO Ph.D ( ICT, Mumbai) , INDIA 25Yrs Exp. in the feld of Organic Chemistry,Working for GLENMARK GENERICS at Navi Mumbai, INDIA. Serving chemists around the world. Helping them with websites on Chemistry.Million hits on google, world acclamation from industry, academia, drug authorities for websites, blogs and educational contribution
Showing posts with label 9. Show all posts
Showing posts with label 9. Show all posts

Wednesday 27 July 2016

4,6,7,8,9,10-hexahydro-1H-6,10-methanopyrazino[2,3-h][3]benzazepine-2,3-dione.



An external file that holds a picture, illustration, etc. Object name is scipharm-2012-80-329f2.jpg



Chemical structures of Varenicline Tartrate and degradant product (DP-I).........4,6,7,8,9,10-hexahydro-1H-6,10-methanopyrazino[2,3-h][3]benzazepine-2,3-dione.
An external file that holds a picture, illustration, etc. Object name is scipharm-2012-80-329f4.jpg
(A) 1H NMR spectrum of DP-I. (B) Proton decoupled 13C NMR spectrum of DP-I.

An external file that holds a picture, illustration, etc. Object name is scipharm-2012-80-329f5.jpg
UHPLC-ToF MS+ of DP-I.


The impurity obtained as pale white crystals. mp 71–73. 
RP-UHPLC, tR = 1.8 min (98.5% purity).

MS (ESI, 70 eV): [M + H+] m/z 244. 

FT-IR (KBr), v, cm−1 3371, 3319, 3279, 3173, 3005, 2808, 1696, 1678, 1588, 1406, 1388, 1338, 1305, 1264, 1135, 1067, 873, 790, 680, 569, 485.

1H NMR (400 MHz, DMSO-d6 +D2O, TMS): δ 7.2 (s, 2H, H-7,8), 3.1–3.4 (m, 6H, H-11,13,14 & 16),2.3 (m, 1H, H-12), 2.0 (d, 1H, 11.2 Hz, H-12).

13C NMR (100 MHz, DMSO-d6, TMS): δ 173.8 (C-2,3), 155.1 (C-5,6), 137.6 (C-9,10), 125.1 (C-7,8), 38.8 (C-11), 37.9 (C-12), 38.8 (C-13), 45.8 (C-14), 48.6 (C-16).

UHPLC ToF MS+: m/z [M + H+].Calcd for C13H13N3O2: 244.1086; found: 244.1082.

Based on the above spectral data, the molecular formula of DP-I is C13H13N3O2 and the corresponding structure was characterized as 4,6,7,8,9,10-hexahydro-1H-6,10-methanopyrazino[2,3-h][3]benzazepine-2,3-dione.
PMC full text:
Published online 2012 Mar 20. doi:  10.3797/scipharm.1201-08
http://dx.doi.org/10.3797/scipharm.1201-08

Saturday 4 July 2015

9,10-Dihydro-9,10-ethanoanthracene-11,12-trans-dicarboxylic acid diethyl ester

9,10-Dihydro-9,10-ethanoanthracene-11,12-trans-dicarboxylic acid diethyl ester

321
Name9,10-Dihydro-9,10-ethanoanthracene-11,12-trans-dicarboxylic acid diethyl ester
Synonyms
Name in Chemical Abstracts9,10-Ethanoanthracene-11,12-dicarboxylic acid, diethyl ester, trans-
CAS No93368-53-7
EINECS No
Molecular formulaC22H22O4
Molecular mass350.42
SMILES codec1cccc2[C@@H]3[C@H](C(=O)OCC)[C@@H](C(=O)OCC)[C@H](c12)c4ccccc43
1H NMR
1H NMR
1H-NMR: 9,10-Dihydro-9,10-ethanoanthracene-11,12-trans-dicarboxylic acid diethyl ester
250 MHz, CDCl3
delta [ppm]mult.atomsassignment
1.23t (3J = 7.2 Hz)6 HCH3 ethyl
3.45m2 H11-H, 12-H (-CH-COO-)
4.08m4 HCH2 ethyl
4.75m2 H9-H, 10-H

13C-NMR

13C NMR
13C-NMR: 9,10-Dihydro-9,10-ethanoanthracene-11,12-trans-dicarboxylic acid diethyl ester
62.5 MHz, CDCl3
delta [ppm]assignment
14.2CH3 (ethyl ester)
46.7C9, C10 (CH)
47.7C11, C12 (CH-COO)
60.9CH2 (ethyl ester)
123.8CH arom.
124.5CH arom.
126.2CH arom.
126.3CH arom.
140.3C quart. arom.
142.0C quart. arom.
172.3C(=O)O-
76.5-77.5CDCl3

IR
IR
IR: 9,10-Dihydro-9,10-ethanoanthracene-11,12-trans-dicarboxylic acid diethyl ester
[KBr, T%, cm-1]
[cm-1]assignment
3074, 3026arom. C-H valence
2981aliph. C-H valence
2935, 2897aliph. C-H valence
1739C=O valence, ester
1467arom. C=C valence


Anthracene+Fumaric acid diethyl ester
reacts to
9,10-Dihydro-9,10-ethanoanthracene-11,12-trans-dicarboxylic acid diethyl ester; Side reactions

Synthesis of 9,10-dihydro-9,10-ethanoanthracene-11,12-trans-dicarboxylic acid diethyl ester

Reaction type:cycloaddition, Diels-Alder reaction
Substance classes:alkene, aromatics, carboxylic acid ester, diene, dienophile, acid catalyst
Techniques:working with moisture exclusion, heating under reflux, stirring with magnetic stir bar, filtering, evaporating with rotary evaporator, recrystallizing, use of an ice cooling bath, heating with oil bath

Equipment

Batch scale:0.01 mol0.1 molAnthracene
three-necked flask 1000 mLthree-necked flask 1000 mLadapter with ground-glass joint and hose couplingadapter with ground-glass joint and hose coupling
protective gas pipingprotective gas pipingreflux condenserreflux condenser
drying tubedrying tubebubble counterbubble counter
powder funnelpowder funnelheatable magnetic stirrer with magnetic stir barheatable magnetic stirrer with magnetic stir bar
rotary evaporatorrotary evaporatorice bathice bath
exsiccator with drying agentexsiccator with drying agentoil bathoil bath

Operating scheme

Operating scheme

MULTAN, PAKISTAN


The multan city of saints
Mutlan is an important city of Pakistan which is also known as the city of Saints. The history of Multan begins with the Alexander and later on Kushans, Arabs, Huns, Ghaznavi, Afghans, Mongols, Sikhs, Mughals and British ruled over the city. It is the city of Sufis and Saints who preached the Islam in this region. In the South Asia Multan is the oldest city.
.

Map of Multan















Multan Things to Do

 See all 10 Things to Do in Multan
  • Baha-ud-din Zakariya Mazar, Multan

    Baha-ud-din Zakariya Mazar

    Sheikh Baha-ud-din Zakariya (1170-1267) was a sufi saint who for several years travelled the region from Baghdad, Iraq to India preaching Islam, and made his final abode in Multan. His offsprings and disciples travelled all over India to preach. His most famous descendant is Shah...  more

  • Shah Rukn-e-Alam's tomb, Multan

    Shah Rukn-e-Alam's tomb

    Situated on top of a small hillock, behind the old ruins of Multan Fort, the Mazar and its majestic dome is the first landmark visible when you enter proper Multan. Shah Rukn-e-Alam (1251-1335) was a Sufi saint in Multan. He was revered by his followers, and to this date thousands of pilgrims from all over...  more

  • Other Saints and Sufis Mazars, Multan

    Other Saints and Sufis Mazars

    Multan is known as City of Saints, and this is evident by the number of Masuleums, Mazars, Dargas, or tombs situated in this city. Some of them are listed below.1 Hazrat Baha-ud-Din Zakaria2 Shah Rukn-i-Alam3 Shah Shams Sabzwari4 Shah Gardez5 Musa Pak Shaheed6 Hazrat Hafiz Muhammad...  more

  • Ghanta Ghar (Clock Tower house), Multan

    Ghanta Ghar (Clock Tower house)

    Ghanta Ghar whch is situated in the city center is the city government head quarter. (not a great picture, taken from a moving car)
     more

  • Multan Fort, Multan

    Multan Fort

    The Multan Fort on a high mound of earth which separated it from the old branch of the river Ravi. There are now only remnant of this old fort, which was considered as one of the best fort (defense wise) built in the sub-continent. The fort was destroyed when the British took over. During its haydays the fort walls were was almost 1.6...  more

  • King mosque Eid Gah, Multan

    King mosque Eid Gah

    This Masjid is a marvelous piece of architecture of multan.it is a very beautiful masjid and must to visit place of Multran city
     more

  • Shrines must to visit, Multan

    Shrines must to visit

    Given below is list of must to visit shrines in Multan1.Shrine B.B Pak Damman2.Shrine Hameed-ud-Din Hakim3.Shrine Qutab-al-quteeb'Moj Daryan'4.Shrine-Syed Pir Sakhi Shah Hasan Prwana5.Shrine-Qazi Qutab-ud-Din Kashani6.Shrine-Syed Hasan Kanjzee7.Shrine-Hazarat Shah Dana Shaheed8.Shrine-Abu...  more

  • Shrines of the sufi hermits, Multan

    Shrines of the sufi hermits

    Hi Awais,All the destinations in Pakistan, they've their own attraction or somethijng very special in that area, likewise in Hunza, you can't find the shrines of the sufi hermits, or in Multan, the mountains like Nanga parbat or Kalash tribes in Lahore?Multan, Medina-tul-awlia, the city of saints, famous all over the...  more

  • Visiting Historical Places, Multan

    Visiting Historical Places

    As I describe before that Multan is the city of Saints so there r so many Tombs to Visit and explore the history.
     more

 Multan Hotels

////////

  DRUG APPROVALS BY DR ANTHONY MELVIN CRASTO .....FOR BLOG HOME CLICK HERE


Join me on Linkedin

View Anthony Melvin Crasto Ph.D's profile on LinkedIn

Join me on Facebook FACEBOOK
Join me on twitterFollow amcrasto on Twitter
Join me on google plus Googleplus

 amcrasto@gmail.com