Sodium Hydroxide → 6-Oxo-7,8,9,10-tetrahydro-6H-pyrido[3',2':4,5]pyrrolo[1,2-a][1,4]diazepine-2-carboxylic acid

HRID 1521702ノート

反応式

HRID 1521702 の反応式
[O:1]=[C:2]1[NH:8][CH2:7][CH2:6][CH2:5][N:4]2[C:9]3[N:15]=[C:14]([C:16]([O:18]CC)=[O:17])[CH:13]=[CH:12][C:10]=3[CH:11]=[C:3]12.[OH-].[Na+]>C(O)C>[O:1]=[C:2]1[NH:8][CH2:7][CH2:6][CH2:5][N:4]2[C:9]3[N:15]=[C:14]([C:16]([OH:18])=[O:17])[CH:13]=[CH:12][C:10]=3[CH:11]=[C:3]12

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 672367606H-Pyrido[3a(2),2a(2):4,5]pyrrolo[1,2-a][1,4]diazepine-2-carboxylic acid, 7,8,9,10-tetrahydro-6-oxo-, ethyl ester

生成物 1

HCID 672363426-Oxo-7,8,9,10-tetrahydro-6H-pyrido[3',2':4,5]pyrrolo[1,2-a][1,4]diazepine-2-carboxylic acid収率 84.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
50 °C

実験手順

To a solution of ethyl 6-oxo-7,8,9,10-tetrahydro-6H-pyrido[3′,2′:4,5]pyrrolo[1,2-a][1,4]diazepine-2-carboxylate (1.84 g, 6.73 mmol) in ethanol (30 mL) is added 1N NaOH solution (16.8 mL, 16.8 mmol). The reaction is stirred at 50° C. for 5 h then is cooled to room temperature. The ethanol is removed in vacuo and the aqueous mixture is acidified to pH 5 with 1N hydrochloric acid. The resulting solid is collected by filtration and dried in vacuo at 50° C. to afford the title compound as a tan solid (1.4 g, quantitative). LCMS: 264.63 (M+H+).

後処理

  1. temperaturethen is cooled to room temperature
  2. customThe ethanol is removed in vacuo
  3. filtrationThe resulting solid is collected by filtration
  4. customdried in vacuo at 50° C.

出典と根拠

ORDレコード
ord-29e1cd74c00746dd9ad62ecb64d0dd18
出典データセット
uspto-grants-2015_07
特許番号
US09073926B2

反応ノート

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