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Pyridine → HCID 136352208、化合物

HRID 880168
ノート
印刷プレビュー

反応式

HRID 880168 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 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

生成物 1

HCID 136352208HCID 136352208、化合物収率 73.9%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

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:

後処理

  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

出典と根拠

ORDレコード
ord-8dbe67f2f1bb480fb293ea3ecfdc92dd
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08993565B2

反応ノート

読み込み中…

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