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Hydrochloric Acid → 2-Chloro-11-[beta-(methylamino)ethylthio]dibenzo[b,f]thiepin hydrochloride

HRID 867469
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HRID 867469 반응식
[Cl:1][C:2]1[CH:30]=[CH:29][C:5]2[S:6][C:7]3[CH:28]=[CH:27][CH:26]=[CH:25][C:8]=3[CH:9]=[C:10]([S:11][CH2:12][CH2:13][N:14](C)[C:15](OC3C=CC=CC=3)=O)[C:4]=2[CH:3]=1.[OH-].[K+].Cl>C(O)CO>[ClH:1].[Cl:1][C:2]1[CH:30]=[CH:29][C:5]2[S:6][C:7]3[CH:28]=[CH:27][CH:26]=[CH:25][C:8]=3[CH:9]=[C:10]([S:11][CH2:12][CH2:13][NH:14][CH3:15])[C:4]=2[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 155683262-chloro-11-[beta-(N-methyl-N-phenoxycarbonylamino)ethylthio]dibenzo[b,f]thiepin

생성물 1

HCID 127949572-Chloro-11-[beta-(methylamino)ethylthio]dibenzo[b,f]thiepin hydrochloride

시약·촉매·용매 1

HCID 174Ethylene Glycol용매

실험 절차

A solution of 5.6 g of 2-chloro-11-[β-(N-methyl-N-phenoxycarbonylamino)ethylthio]dibenzo[b,f]thiepin, Example 6, 127 ml of ethylene glycol and 10.8 g of potassium hydroxide is stirred at 150°-155° C. for 30 minutes. Thereafter the reaction mixture is poured onto 300 ml of ice-water and the aqueous mixture is extracted with an ether-toluene (1:1) mixture. The combined extracts, successively, are washed well with water, dried and filtered and the filtrate evaporated leaving an orange oil. The oil is converted to its hydrogen chloride acid salt which is recrystallized from a methanol-acetone-ether mixture to give the product, mp 194°-196° C. of 2-chloro-11-[β-(methylamino)ethylthio]dibenzo[b,f]thiepin hydrochloride..

후처리

  1. extractionthe aqueous mixture is extracted with an ether-toluene (1:1) mixture
  2. washThe combined extracts, successively, are washed well with water
  3. customdried
  4. filtrationfiltered
  5. customthe filtrate evaporated
  6. customleaving an orange oil
  7. customis recrystallized from a methanol-acetone-ether mixture

출처 및 근거

ORD 기록
ord-628d45c6e4674f63adba7efd56c5340c
출처 데이터셋
uspto-grants-1988_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04775683

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