Ammonia → HCID 57965575、化合物

HRID 1798981ノート

反応式

HRID 1798981 の反応式
[F:1][C:2]([F:45])([F:44])[C:3]1[CH:4]=[C:5]([C:13]([CH3:43])([CH3:42])[C:14]([N:16]([CH3:41])[C:17]2[C:18]([C:33]3[CH:38]=[CH:37][C:36]([F:39])=[CH:35][C:34]=3[CH3:40])=[CH:19][C:20]([C:23]3[CH2:24][CH2:25][C@:26]([CH3:32])([C:28](OC)=[O:29])[N:27]=3)=[N:21][CH:22]=2)=[O:15])[CH:6]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:8]=1.[NH3:46]>CO>[F:11][C:9]([F:12])([F:10])[C:7]1[CH:6]=[C:5]([C:13]([CH3:43])([CH3:42])[C:14]([N:16]([CH3:41])[C:17]2[C:18]([C:33]3[CH:38]=[CH:37][C:36]([F:39])=[CH:35][C:34]=3[CH3:40])=[CH:19][C:20]([C:23]3[CH2:24][CH2:25][C@:26]([CH3:32])([C:28]([NH2:46])=[O:29])[N:27]=3)=[N:21][CH:22]=2)=[O:15])[CH:4]=[C:3]([C:2]([F:44])([F:45])[F:1])[CH:8]=1

参加物

4

反応物 2

HCID 222AmmoniaHCID 57965549HCID 57965549、化合物2 回

生成物 1

HCID 57965575HCID 57965575、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
20 °C

実験手順

Methyl (2R)-5-[5-[{2-[3,5-bis(trifluoromethyl)phenyl]-2-methylpropanoyl}(methyl)amino]-4-(4-fluoro-2-methylphenyl)pyridin-2-yl]-2-methyl-3,4-dihydro-2H-pyrrole-2-carboxylate (Intermediate 23 1.06 Kg) was suspended in 20.44 L of 7M ammonia in methanol. The mixture was gently stirred for at least 5 days at 20° C. The mixture was concentrated by half by distillation at atmospheric pressure. The solution obtained was then cooled to 40° C. and stirred for 1 h. The slurry obtained was then cooled to 0° C. over 3 h and aged at 0° C. for 2 h. The title compound was then isolated by filtration and the cake washed with ice cold methanol (1.1 L). The wet cake was dried at 40° C./vacuum to yield the title compound (841.3 g).

後処理

  1. concentrationThe mixture was concentrated by half by distillation at atmospheric pressure
  2. customThe solution obtained
  3. temperaturewas then cooled to 40° C.
  4. stirringstirred for 1 h
  5. customThe slurry obtained
  6. temperaturewas then cooled to 0° C. over 3 h

出典と根拠

ORDレコード
ord-1d68fc3c25d545a9bb78c08991f88d89
出典データセット
uspto-grants-2013_01
特許番号
US08344005B2

反応ノート

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