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Hydrazine hydrate (1:1) → HCID 178501755、化合物

HRID 2037180
ノート
印刷プレビュー

反応式

HRID 2037180 の反応式
[CH3:1][C:2]([CH3:36])([CH3:35])[C:3]([C:5]1[CH:9]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[O:16][CH2:17][C:18]([O:20][CH3:21])=[O:19])[N:8]([C:22]2[CH:27]=[CH:26][C:25]([C:28]3[CH:32]=[CH:31][S:30][CH:29]=3)=[CH:24][CH:23]=2)[C:7](=[O:33])[C:6]=1O)=O.O.[NH2:38][NH2:39].C(=O)(O)[O-].[Na+]>C(O)(=O)C>[C:2]([C:3]1[C:5]2[CH:9]([C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=3[O:16][CH2:17][C:18]([O:20][CH3:21])=[O:19])[N:8]([C:22]3[CH:27]=[CH:26][C:25]([C:28]4[CH:32]=[CH:31][S:30][CH:29]=4)=[CH:24][CH:23]=3)[C:7](=[O:33])[C:6]=2[NH:38][N:39]=1)([CH3:36])([CH3:35])[CH3:1]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 24654Hydrazine hydrate (1:1)HCID 516892Sodium BicarbonateHCID 583653294-(2,2-Dimethylpropionyl)-3-hydroxy-5-(2-methoxycarbonylmethyloxyphenyl)-1-(4-thiophene-3-ylphenyl)-1,5-dihydropyrrole-2-one

生成物 1

HCID 178501755HCID 178501755、化合物収率 93%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
95 °C

実験手順

A mixture of 4-(2,2-dimethylpropionyl)-3-hydroxy-5-(2-methoxycarbonylmethyloxyphenyl)-1-(4-thiophene-3-ylphenyl)-1,5-dihydropyrrole-2-one (0.207 g, 0.41 mmol), hydrazine hydrate (0.022 mL, 0.45 mmol) and acetic acid (3.1 mL) was stirred at 95° C. for 1 hour. After the reaction was completed, saturated sodium bicarbonate solution was poured into the reaction mixture, and the mixture was extracted with chloroform. The extract was washed with brine, dried over anhydrous sodium sulphate, and then concentrated in vacuo. The resulting residue was triturated with ethyl ether and diisopropyl ether to give 3-t-butyl-5-(4-thiophene-3-ylphenyl)-4-(2-methoxycarbonylmethyloxyphenyl)-4,5-dihydro-1H-pyrrolo[3,4-c]pyrazole-6-one (0.191 g, yield: 93%) as pale brown solid.

後処理

  1. extractionthe mixture was extracted with chloroform
  2. washThe extract was washed with brine
  3. dry with materialdried over anhydrous sodium sulphate
  4. concentrationconcentrated in vacuo
  5. customThe resulting residue was triturated with ethyl ether and diisopropyl ether

出典と根拠

ORDレコード
ord-7fb90f61bbd44758a3f72a5f0f8a8d8a
出典データセット
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08575197B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート