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Pyridine → HCID 136352208, 화합물

HRID 880168
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HRID 880168 반응식
N1C=CC=CC=1.Cl.CN(C)CCCN=C=NCC.[S:19]1[CH:23]=[CH:22][C:21]2[C:24]([NH2:28])=[CH:25][CH:26]=[CH:27][C:20]1=2.[N:29]1([C:35]2[N:36]=[C:37]([CH2:42][C:43]([O-])=[O:44])[NH:38][C:39](=[O:41])[CH:40]=2)[CH2:34][CH2:33][O:32][CH2:31][CH2:30]1.[Na+]>CN(C)C=O>[S:19]1[C:20]2[CH:27]=[CH:26][CH:25]=[C:24]([NH:28][C:43](=[O:44])[CH2:42][C:37]3[NH:38][C:39](=[O:41])[CH:40]=[C:35]([N:29]4[CH2:34][CH2:33][O:32][CH2:31][CH2:30]4)[N:36]=3)[C:21]=2[CH:22]=[CH:23]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 1049PyridineHCID 298484Benzo(b)thiophen-4-ylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 136041844Sodium (4-morpholin-4-yl-6-oxo-1,6-dihydropyrimidin-2-yl)acetate

생성물 1

HCID 136352208HCID 136352208, 화합물수율 73.9%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

2 ml of pyridine, 257 mg of N-[3-(dimethylamino)propyl]-N′-ethylcarbodiimide hydrochloride and 223 mg of benzo[B]thiophen-4-ylamine are added to a solution of 250 mg of sodium [4-(morpholin-4-yl)-6-oxo-1,6-dihydropyrimidin-2-yl]acetate prepared in stage 2 of example 1, in 2 ml of N,N-dimethylformamide. The reaction mixture is stirred at ambient temperature for 15 hours, and then concentrated under reduced pressure. Water and ethyl acetate are added and the resulting mixture is thus stirred for 30 minutes. The precipitate formed is filtered off, and rinsed with water, ethyl ether and petroleum ether. The solid obtained is dried under vacuum. 262 mg of N-(1-benzothiophen-4-yl)-2-[4-(morpholin-4-yl)-6-oxo-1,6-dihydropyrimidin-2-yl]acetamide are obtained in the formed of an off-white solid, the characteristics of which are the following:

후처리

  1. concentrationconcentrated under reduced pressure
  2. additionWater and ethyl acetate are added
  3. stirringthe resulting mixture is thus stirred for 30 minutes
  4. customThe precipitate formed
  5. filtrationis filtered off
  6. washrinsed with water, ethyl ether and petroleum ether
  7. customThe solid obtained
  8. customis dried under vacuum

출처 및 근거

ORD 기록
ord-8dbe67f2f1bb480fb293ea3ecfdc92dd
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08993565B2

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