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Water → HCID 21472076, 화합물

HRID 1734063
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HRID 1734063 반응식
[S:1]1[C:5]2[C:6](=[O:11])[NH:7][CH2:8][CH2:9][CH2:10][C:4]=2[CH:3]=[CH:2]1.[Cl:12][CH2:13][C:14](Cl)=[O:15].[Cl-].[Al+3].[Cl-].[Cl-].O>ClCCl>[Cl:12][CH2:13][C:14]([C:2]1[S:1][C:5]2[C:6](=[O:11])[NH:7][CH2:8][CH2:9][CH2:10][C:4]=2[CH:3]=1)=[O:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 6577Chloroacetyl chlorideHCID 6451240Aluminum(III) ChlorideHCID 21471822HCID 21471822, 화합물

생성물 1

HCID 21472076HCID 21472076, 화합물수율 68.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 2 g of 4,5,6,7-tetrahydro-8H-thieno[2,3-c]azepin-8-one and 2 g of chloroacetyl chloride in 25 ml of dichloromethane was added 4.8 g of aluminum chloride. The mixture was stirred for 30 minutes, refluxed under heating for an hour and then poured into water. The precipitated crystals were collected by filtration and washed with isopropyl alcohol to give 2 g of 2-chloroacetyl-4,5,6,7-tetrahydro-8H-thieno[2,3-c]azepin-8-one, m.p. 221°-223° C. (decomposition).

후처리

  1. temperaturerefluxed
  2. temperatureunder heating for an hour
  3. filtrationThe precipitated crystals were collected by filtration
  4. washwashed with isopropyl alcohol

출처 및 근거

ORD 기록
ord-52e62c26e2204f79892617b06b6942e6
출처 데이터셋
uspto-grants-1996_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05532240

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