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

HRID 1973092ノート

反応式

HRID 1973092 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b7eaea481e3543b987b488cc751ca4f4
出典データセット
uspto-grants-1976_12
特許番号
US03996229

反応ノート

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