Diethyl Ether → (R)-1-(Pyrazin-2-ylcarbamoylmethyl)-3-(1-thiophen-2-yl-cycloheptanecarbonyloxy)-1-azonia-bicyclo[2.2.2]octane bromide

HRID 2192320ノート

反応式

HRID 2192320 の反応式
[N:1]12[CH2:8][CH2:7][CH:4]([CH2:5][CH2:6]1)[C@@H:3]([O:9][C:10]([C:12]1([C:19]3[S:20][CH:21]=[CH:22][CH:23]=3)[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]1)=[O:11])[CH2:2]2.[Br:24][CH2:25][C:26]([NH:28][C:29]1[CH:34]=[N:33][CH:32]=[CH:31][N:30]=1)=[O:27].C(OCC)C.CCCC(C)C>C(#N)C>[Br-:24].[N:30]1[CH:31]=[CH:32][N:33]=[CH:34][C:29]=1[NH:28][C:26]([CH2:25][N+:1]12[CH2:6][CH2:5][CH:4]([CH2:7][CH2:8]1)[C@@H:3]([O:9][C:10]([C:12]1([C:19]3[S:20][CH:21]=[CH:22][CH:23]=3)[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]1)=[O:11])[CH2:2]2)=[O:27]

参加物

6

反応物 4

HCID 3283Diethyl EtherHCID 78922-MethylpentaneHCID 445426692-bromo-N-(pyrazin-2-yl)acetamideHCID 58348375HCID 58348375、化合物

生成物 1

HCID 44516990(R)-1-(Pyrazin-2-ylcarbamoylmethyl)-3-(1-thiophen-2-yl-cycloheptanecarbonyloxy)-1-azonia-bicyclo[2.2.2]octane bromide

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

1-Thiophen-2-yl-cycloheptanecarboxylic acid (R)-(1-aza-bicyclo[2.2.2]oct-3-yl)ester (Example 5d) (116 mg) and 2-bromo-N-pyrazin-2-yl-acetamide (Example 11a) (75 mg were dissolved in acetonitrile (2 mL) and left overnight. Diethyl ether (10 mL) and isohexane (8 mL) were added and the mixture was left to stand overnight. The resulting crystals were filtered off and washed with diethyl ether to afford the titled compound (117 mg).

後処理

  1. waitthe mixture was left
  2. waitto stand overnight
  3. filtrationThe resulting crystals were filtered off
  4. washwashed with diethyl ether

出典と根拠

ORDレコード
ord-b826ddab0f2d43f5ae29ddb5dc7c5c4e
出典データセット
uspto-grants-2012_12
特許番号
US08329729B2

反応ノート

読み込み中…