Lithium hydroxide, monohydrate → Lithium 7-(4-(2-(1-acetylindolin-5-yl)ethyl)piperazin-1-yl)benzofuran-2-carboxylate

HRID 383823

反応式

HRID 383823 の反応式
O.[OH-].[Li+:3].[C:4]([N:7]1[C:15]2[C:10](=[CH:11][C:12]([CH2:16][CH2:17][N:18]3[CH2:23][CH2:22][N:21]([C:24]4[C:32]5[O:31][C:30]([C:33]([O:35]CC)=[O:34])=[CH:29][C:28]=5[CH:27]=[CH:26][CH:25]=4)[CH2:20][CH2:19]3)=[CH:13][CH:14]=2)[CH2:9][CH2:8]1)(=[O:6])[CH3:5]>O1CCCC1.O>[C:4]([N:7]1[C:15]2[C:10](=[CH:11][C:12]([CH2:16][CH2:17][N:18]3[CH2:19][CH2:20][N:21]([C:24]4[C:32]5[O:31][C:30]([C:33]([O-:35])=[O:34])=[CH:29][C:28]=5[CH:27]=[CH:26][CH:25]=4)[CH2:22][CH2:23]3)=[CH:13][CH:14]=2)[CH2:9][CH2:8]1)(=[O:6])[CH3:5].[Li+:3]

参加物

5

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 59636756Ethyl 7-(4-(2-(1-acetylindolin-5-yl)ethyl)piperazin-1-yl)benzofuran-2-carboxylate

生成物 1

HCID 66847495Lithium 7-(4-(2-(1-acetylindolin-5-yl)ethyl)piperazin-1-yl)benzofuran-2-carboxylate収率 99.3%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
100 °C

実験手順

Lithium hydroxide monohydrate (0.087 g, 2.08 mmol) was added to a solution of ethyl 7-(4-(2-(1-acetylindolin-5-yl)ethyl)piperazin-1-yl)benzofuran-2-carboxylate (0.481 g, 1.04 mmol) in tetrahydrofuran (9 mL) and water (1 mL) and the reaction was heated at 100° C. for 35 min in a microwave oven. The solvents were evaporated and the material was dried in vacuum over P2O5 to give 0.454 g of the crude product. The crude material was used in the next step assuming quantitative yield without further purification. MS (ES+) m/z 434.2 (M+H)+.

後処理

  1. customThe solvents were evaporated
  2. dry with materialthe material was dried in vacuum over P2O5

出典と根拠

ORDレコード
ord-130c86dc8d8f40b6bb24f227a30ab921
出典データセット
uspto-grants-2013_02
特許番号
US08367676B2

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