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Water → HCID 21471762, 화합물

HRID 2294841
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HRID 2294841 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][CH2:14][CH2:15][C:16](Cl)=[O:17].[Cl-].[Al+3].[Cl-].[Cl-].O>ClCCl>[Cl:12][CH2:13][CH2:14][CH2:15][C:16]([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:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 783704-Chlorobutyryl chlorideHCID 6451240Aluminum(III) ChlorideHCID 21471822HCID 21471822, 화합물

생성물 1

HCID 21471762HCID 21471762, 화합물수율 36.9%

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 2.5 g of 4-chlorobutyryl chloride in 25 ml of dichloromethane was added 4.8 g of aluminum chloride under cooling. The mixture was stirred for 80 minutes, refluxed under heating and poured into water, and then extracted with chloroform. The extract was washed with water, dried over magnesium sulfate and concentrated. The residue was crystallized from ethyl acetate-isopropyl ether to give 1.2 g of 2-(4-chlorobutyryl)-4,5,6,7-tetrahydro-8H-thieno[2,3-c]azepin-8-one as white crystals, m.p. 163°14 165° C.

후처리

  1. temperatureunder cooling
  2. temperaturerefluxed
  3. temperatureunder heating
  4. extractionextracted with chloroform
  5. washThe extract was washed with water
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated
  8. customThe residue was crystallized from ethyl acetate-isopropyl ether

출처 및 근거

ORD 기록
ord-1f5f5db0934a489dad5c53cbd29881d6
출처 데이터셋
uspto-grants-1997_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05691330

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