2-Bromo-N-(3,5-difluorophenyl)acetamide → HCID 53311178、化合物

HRID 2192360ノート

反応式

HRID 2192360 の反応式
[Br:1][CH2:2][C:3]([NH:5][C:6]1[CH:11]=[C:10]([F:12])[CH:9]=[C:8]([F:13])[CH:7]=1)=[O:4].[N:14]12[CH2:21][CH2:20][CH:17]([CH2:18][CH2:19]1)[C@@H:16]([O:22][C:23]([C:25]1([C:32]3[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=3)[CH2:31][CH2:30][CH2:29][CH2:28][CH2:27][CH2:26]1)=[O:24])[CH2:15]2>CC#N>[Br-:1].[F:13][C:8]1[CH:7]=[C:6]([NH:5][C:3]([CH2:2][N+:14]23[CH2:21][CH2:20][CH:17]([CH2:18][CH2:19]2)[C@@H:16]([O:22][C:23]([C:25]2([C:32]4[CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=4)[CH2:31][CH2:30][CH2:29][CH2:28][CH2:27][CH2:26]2)=[O:24])[CH2:15]3)=[O:4])[CH:11]=[C:10]([F:12])[CH:9]=1

参加物

4

反応物 2

HCID 231521612-Bromo-N-(3,5-difluorophenyl)acetamideHCID 591796191-Phenyl-cycloheptanecarboxylic acid (R)-(1-aza-bicyclo[2.2.2]oct-3-yl)ester

生成物 1

HCID 53311178HCID 53311178、化合物収率 17%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A mixture of 2-bromo-N-(3,5-difluoro-phenyl)-acetamide (42 mg) (Example 35a) and 1-phenyl-cycloheptanecarboxylic acid (R)-(1-aza-bicyclo[2.2.2]oct-3-yl)ester (Example 14e) (50 mg) in MeCN (1 mL) was stirred at room temperature for 72 h. The solid precipitate was filtered off, washed with ether and dried at 50° C. under vacuum overnight. The mother liquors were evaporated, treated with ether and the resulting solid was filtered off. The solids were combined and crystallised from hot isopropyl alcohol to give the title compound (15 mg) as a colourless solid.

後処理

  1. filtrationThe solid precipitate was filtered off
  2. washwashed with ether
  3. customdried at 50° C. under vacuum overnight
  4. customThe mother liquors were evaporated
  5. additiontreated with ether
  6. filtrationthe resulting solid was filtered off
  7. customcrystallised from hot isopropyl alcohol

出典と根拠

ORDレコード
ord-40cec1d02a0d40d8958b2d3d407ec4cd
出典データセット
uspto-grants-2012_12
特許番号
US08329729B2

反応ノート

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