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5-Chlorovaleryl chloride → HCID 13656413, 화합물

HRID 579755
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인쇄 미리보기

반응식

HRID 579755 반응식
[NH2:1][CH:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[CH2:6][S:5][C:4]2[CH:13]=[CH:14][CH:15]=[CH:16][C:3]1=2.[Cl:17][CH2:18][CH2:19][CH2:20][CH2:21][C:22](Cl)=[O:23]>O1CCOCC1>[Cl:17][CH2:18][CH2:19][CH2:20][CH2:21][C:22]([NH:1][CH:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[CH2:6][S:5][C:4]2[CH:13]=[CH:14][CH:15]=[CH:16][C:3]1=2)=[O:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 740895-Chlorovaleryl chlorideHCID 124891006,11-Dihydrodibenzo[b,e]thiepin-11-amine

생성물 1

HCID 13656413HCID 13656413, 화합물수율 93.4%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A mixture of 8.8 g of 11-amino-6,11-dihydrodibenzo[b,e]thiepin, 6.0 g of 5-chlorovaleryl chloride and 100 ml of dioxane is heated with stirring under reflux for 15 hours. The solvent is distilled off under reduced pressure. The residue is recrystallized from ethanol to give 12.5 g of the title compound, m.p. 155°-156° C.

후처리

  1. temperatureis heated
  2. temperatureunder reflux for 15 hours
  3. distillationThe solvent is distilled off under reduced pressure
  4. customThe residue is recrystallized from ethanol

출처 및 근거

ORD 기록
ord-803d42ff85124d48bb7b648bf79a6341
출처 데이터셋
uspto-grants-1988_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04749703

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