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Acetic Anhydride → HCID 11375081, 화합물

HRID 1271070
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HRID 1271070 반응식
C(N(CC)CC)C.C(O[C:12](=[O:14])[CH3:13])(=O)C.[Cl:15][C:16]1[CH:46]=[CH:45][C:19]([CH2:20][N:21]2[C:29]3[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=3)[C:23]([C:30](=[O:44])[C:31]([NH:33][C:34]3[CH:35]=[C:36]4[C:41](=[CH:42][CH:43]=3)[N:40]=[CH:39][CH:38]=[CH:37]4)=[O:32])=[CH:22]2)=[CH:18][CH:17]=1.C(OCC)(=O)C>CN(C1C=CN=CC=1)C.CN(C=O)C.O>[Cl:15][C:16]1[CH:17]=[CH:18][C:19]([CH2:20][N:21]2[C:29]3[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=3)[C:23]([C:30](=[O:44])[C:31]([N:33]([C:34]3[CH:35]=[C:36]4[C:41](=[CH:42][CH:43]=3)[N:40]=[CH:39][CH:38]=[CH:37]4)[C:12](=[O:14])[CH3:13])=[O:32])=[CH:22]2)=[CH:45][CH:46]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 10203597Entasobulin

생성물 1

HCID 11375081HCID 11375081, 화합물

시약·촉매·용매 3

HCID 142844-(Dimethylamino)pyridine촉매
HCID 962
Water
용매
HCID 6228Dimethylformamide용매

실험 절차

0.833 g (6.82 mMol) of DMAP, 1.38 g (13.6 mMol) of triethylamine and 13.9 g (136 mMol) of acetic anhydride are added, under nitrogen, to a stirred solution of 6.0 g (13.6 mMol) of 2-[1-(4-chlorobenzyl)-1H-indol-3-yl]-2-oxo-N-quinolin-6-ylacetamide in 60 ml of DMF. The reaction mixture is stirred at room temperature for 10 minutes and, after that, poured into 200 ml of ethyl acetate. After 300 ml of water have been added, the mixture is shaken in a separating funnel after which the two phase separate. Precipitation begins after 20 minutes. The pale yellow crystals are filtered off and dried in vacuo at 60° C.

후처리

  1. stirringthe mixture is shaken in a separating funnel after which the two phase
  2. customseparate
  3. customPrecipitation
  4. waitbegins after 20 minutes
  5. filtrationThe pale yellow crystals are filtered off
  6. customdried in vacuo at 60° C.

출처 및 근거

ORD 기록
ord-cd002fb98cc54947b11cb988e0813ee5
출처 데이터셋
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07205299B2

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