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

HRID 1788938
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HRID 1788938 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 138218607-Chloro-3-hydroxymethyl-2-methylimidazo[2,1-a]isoquinoline

생성물 1

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

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-1dc58f9bdebb49a9ac8f93e49b2889db
출처 데이터셋
uspto-grants-1987_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04686227

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