Hydrochloric Acid → 10-Chloro-10,11-dihydro-3-methoxy-8-methylthio-dibenzo[b,f]thiepin

HRID 1973092노트

반응식

HRID 1973092 반응식
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[CH2:12][CH:11](O)[C:10]3[CH:14]=[C:15]([S:18][CH3:19])[CH:16]=[CH:17][C:9]=3[S:8][C:7]=2[CH:20]=1.[Cl-:21].[Ca+2].[Cl-].Cl>C1C=CC=CC=1>[Cl:21][CH:11]1[C:10]2[CH:14]=[C:15]([S:18][CH3:19])[CH:16]=[CH:17][C:9]=2[S:8][C:7]2[CH:20]=[C:3]([O:2][CH3:1])[CH:4]=[CH:5][C:6]=2[CH2:12]1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 5284359Calcium ChlorideHCID 1282219810,11-Dihydro-3-methoxy-8-methylthio-dibenzo[b,f]thiepin-10-ol

생성물 1

HCID 1282220110-Chloro-10,11-dihydro-3-methoxy-8-methylthio-dibenzo[b,f]thiepin

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

15.7 G. of 10,11-dihydro-3-methoxy-8-methylthio-dibenzo[b,f]thiepin-10-ol, 250 ml. of benzene and 6 g. of finely powdered calcium chloride are saturated with hydrogen chloride gas at 15° C. within 2.5 hours and then stirred for an additional 3 hours. After the addition of 0.8 g. of active carbon, the precipitate is removed by filtration and washed with benzene. The benzene phase is evaporated under reduced pressure, and there is obtained 10-chloro-10,11-dihydro-3-methoxy-8-methylthio-dibenzo[b,f]thiepin having a melting point of 120°-123° C.

후처리

  1. additionAfter the addition of 0.8 g
  2. customof active carbon, the precipitate is removed by filtration
  3. washwashed with benzene
  4. customThe benzene phase is evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-b7eaea481e3543b987b488cc751ca4f4
출처 데이터셋
uspto-grants-1976_12
특허 번호
US03996229

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