Sodium Hydroxide → 3-{3-[4-(diphenylmethyl)-1-piperazinyl]-propyl}-2,3-dihydro-2-oxo-1H-benzimidazole-1-acetic acid hemihydrate

HRID 1413535

反応式

HRID 1413535 の反応式
[C:1]1([CH:7]([C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)[N:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][CH2:16][N:17]3[C:21]4[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=4[N:19]([CH2:26][C:27]([O:29]CC)=[O:28])[C:18]3=[O:32])[CH2:10][CH2:9]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[OH-].[Na+]>O>[OH2:28].[C:33]1([CH:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[N:8]2[CH2:9][CH2:10][N:11]([CH2:14][CH2:15][CH2:16][N:17]3[C:21]4[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=4[N:19]([CH2:26][C:27]([OH:29])=[O:28])[C:18]3=[O:32])[CH2:12][CH2:13]2)[CH:34]=[CH:35][CH:36]=[CH:37][CH:38]=1.[C:1]1([CH:7]([N:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][CH2:16][N:17]3[C:21]4[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=4[N:19]([CH2:26][C:27]([OH:29])=[O:28])[C:18]3=[O:32])[CH2:10][CH2:9]2)[C:33]2[CH:34]=[CH:35][CH:36]=[CH:37][CH:38]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 20506279ethyl 3-{3-[4-(diphenylmethyl)-1-piperazinyl]propyl}-2,3-dihydro-2-oxo-1H-benzimidazole-1-acetate

生成物 1

HCID 887389743-{3-[4-(diphenylmethyl)-1-piperazinyl]-propyl}-2,3-dihydro-2-oxo-1H-benzimidazole-1-acetic acid hemihydrate

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

A mixture of 9.8 parts of ethyl 3-{3-[4-(diphenylmethyl)-1-piperazinyl]propyl}-2,3-dihydro-2-oxo-1H-benzimidazole-1-acetate, 1.2 parts of sodium hydroxide and 150 parts of water is stirred and refluxed for 5 minutes (±80° C.). The reaction mixture is filtered and the filtrate is acidified with acetic acid to pH 5.8-6: a sticky precipitate is formed. It is separated and crystallized from ethanol and water. The product is filtered off and dried in vacuo at 100° C. for 3 hours, yielding 6 parts 3-{3-[4-(diphenylmethyl)-1-piperazinyl]-propyl}-2,3-dihydro-2-oxo-1H-benzimidazole-1-acetic acid hemihydrate; mp. 138.7° C.

後処理

  1. filtrationThe reaction mixture is filtered
  2. customa sticky precipitate is formed
  3. customIt is separated
  4. customcrystallized from ethanol and water
  5. filtrationThe product is filtered off
  6. customdried in vacuo at 100° C. for 3 hours

出典と根拠

ORDレコード
ord-a181925ced044850bc05a0b102384d67
出典データセット
uspto-grants-1981_02
特許番号
US04250176

関連ノート

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