4-Chlorobutyryl chloride → 7-(4-chlorobutyryl)-2,3-dihydrothieno[3,2-f][1,4]thiazepin-5(4H)-one

HRID 2294806노트

반응식

HRID 2294806 반응식
[S:1]1[C:7]2[S:8][CH:9]=[CH:10][C:6]=2[C:5](=[O:11])[NH:4][CH2:3][CH2:2]1.[Cl:12][CH2:13][CH2:14][CH2:15][C:16](Cl)=[O:17].[Cl-].[Al+3].[Cl-].[Cl-]>ClC(Cl)C>[Cl:12][CH2:13][CH2:14][CH2:15][C:16]([C:9]1[S:8][C:7]2[S:1][CH2:2][CH2:3][NH:4][C:5](=[O:11])[C:6]=2[CH:10]=1)=[O:17]

참가 물질

5

반응물 3

HCID 783704-Chlorobutyryl chlorideHCID 43659423,4-dihydrothieno[3,2-f][1,4]thiazepin-5(2H)-oneHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 214720567-(4-chlorobutyryl)-2,3-dihydrothieno[3,2-f][1,4]thiazepin-5(4H)-one수율 59%

시약·촉매·용매 1

HCID 63651,1-Dichloroethane용매

실험 절차

To a mixture of 13 g of 2,3-dihydrothieno[3,2-f][1,4]thiazepin-5(4H)-one and 21.5 g of 4-chlorobutyryl chloride in 200 ml of dichloroethane was added 21.5 g of aluminum chloride under cooling and the mixture was stirred for 3 hours. The mixture was poured into ice-cold water and extracted with chloroform. The organic layer was washed with saline solution, dried over magnesium sulfate and concentrated. The residue was recrystallized from ethanol to give 12 g of 7-(4-chlorobutyryl)-2,3-dihydrothieno[3,2-f][1,4]thiazepin-5(4H)-one as white crystals, m.p. 124°-125° C.

후처리

  1. temperatureunder cooling
  2. additionThe mixture was poured into ice-cold water
  3. extractionextracted with chloroform
  4. washThe organic layer was washed with saline solution
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated
  7. customThe residue was recrystallized from ethanol

출처 및 근거

ORD 기록
ord-4fe21fffeb3b499886d0dd311c14643d
출처 데이터셋
uspto-grants-1997_11
특허 번호
US05691330

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