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Potassium Hydroxide → HCID 70817365、化合物

HRID 82217
ノート
印刷プレビュー

反応式

HRID 82217 の反応式
[OH-].[K+].[Cl:3][C:4]1[CH:12]=[C:11]2[C:7]([C:8]([CH2:14][C:15]([O:17]CC)=[O:16])=[N:9][N:10]2[CH3:13])=[CH:6][CH:5]=1>CO>[Cl:3][C:4]1[CH:12]=[C:11]2[C:7]([C:8]([CH2:14][C:15]([OH:17])=[O:16])=[N:9][N:10]2[CH3:13])=[CH:6][CH:5]=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

4

反応物 2

HCID 14797Potassium HydroxideHCID 70847731Ethyl (6-chloro-1-methyl-1H-indazol-3-yl)acetate

生成物 1

HCID 70817365HCID 70817365、化合物収率 56%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
25 °C

実験手順

Aqueous potassium hydroxide (5.93 mL, 10%) was added to ethyl (6-chloro-1-methyl-1H-indazol-3-yl)acetate (Preparation 169, 1.78 g, 0.704 mol) in MeOH (30 mL). The mixture was stirred for 1 hour at 25° C. then the methanol was evaporated in vacuo. The aqueous residue was washed with diethyl ether (30 mL) then acidified with aqueous HCl (6 M). The mixture was extracted with ethyl acetate (30 mL) and the organic phase was dried over sodium sulphate, evaporated in vacuo and purified by column chromatography on silica gel (DCM:MeOH 95:5) to afford the title compound as a white solid in 56% yield, 865 mg.

後処理

  1. customthe methanol was evaporated in vacuo
  2. washThe aqueous residue was washed with diethyl ether (30 mL)
  3. extractionThe mixture was extracted with ethyl acetate (30 mL)
  4. dry with materialthe organic phase was dried over sodium sulphate
  5. customevaporated in vacuo
  6. custompurified by column chromatography on silica gel (DCM:MeOH 95:5)

出典と根拠

ORDレコード
ord-26182695954a45acb00e1e49a0ed6aaf
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08846698B2

反応ノート

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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