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Acetic Anhydride → 3-Acetoxymethyl-7-chloro-2-methylimidazo[2,1-a]isoquinoline

HRID 1788938
ノート
印刷プレビュー

反応式

HRID 1788938 の反応式
[C:1]([O:4][C:5](=[O:7])[CH3:6])(=O)[CH3:2].[Cl:8][C:9]1[CH:18]=[CH:17][CH:16]=[C:15]2[C:10]=1[CH:11]=[CH:12][N:13]1[C:21](CO)=[C:20](C)[N:19]=[C:14]12>N1C=CC=CC=1>[C:5]([O:4][CH2:1][C:2]1[N:13]2[CH:12]=[CH:11][C:10]3[C:15]([C:14]2=[N:19][C:20]=1[CH3:21])=[CH:16][CH:17]=[CH:18][C:9]=3[Cl:8])(=[O:7])[CH3:6]
参加物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 7918Acetic AnhydrideHCID 138218607-Chloro-3-hydroxymethyl-2-methylimidazo[2,1-a]isoquinoline

生成物 1

HCID 138218613-Acetoxymethyl-7-chloro-2-methylimidazo[2,1-a]isoquinoline収率 35.8%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

Acetic anhydride (0.71 g) was added dropwise to a suspension of 7-chloro-3-hydroxymethyl-2-methylimidazo[2,1-a]isoquinoline (1.43 g) in pyridine (14 ml) and the mixture was stirred at room temperature for 24 hours. The mixture was evaporated in vacuo and the residue was extracted with chloroform after an addition of water to it. The extract was washed with water, dried over magnesium sulfate, treated with activated charcoal and evaporated in vacuo. The crystalline residue was recrystallized from a mixture of ethyl acetate and diisopropyl ether to give 3-acetoxymethyl-7-chloro-2-methylimidazo[2,1-a]isoquinoline (0.6 g).

後処理

  1. customThe mixture was evaporated in vacuo
  2. extractionthe residue was extracted with chloroform
  3. additionafter an addition of water to it
  4. washThe extract was washed with water
  5. dry with materialdried over magnesium sulfate
  6. additiontreated with activated charcoal
  7. customevaporated in vacuo
  8. customThe crystalline residue was recrystallized from a mixture of ethyl acetate and diisopropyl ether

出典と根拠

ORDレコード
ord-1dc58f9bdebb49a9ac8f93e49b2889db
出典データセット
uspto-grants-1987_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04686227

反応ノート

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