1-Methylpiperazine → HCID 3041883, 화합물

HRID 1658742노트

반응식

HRID 1658742 반응식
[Cl:1][C:2]1[CH:18]=[CH:17][C:5]2[S:6][C:7]3[CH:15]=[C:14]([F:16])[CH:13]=[CH:12][C:8]=3[CH:9](Cl)[CH2:10][C:4]=2[CH:3]=1.[CH3:19][N:20]1[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]1>>[Cl:1][C:2]1[CH:18]=[CH:17][C:5]2[S:6][C:7]3[CH:15]=[C:14]([F:16])[CH:13]=[CH:12][C:8]=3[CH:9]([N:23]3[CH2:24][CH2:25][N:20]([CH3:19])[CH2:21][CH2:22]3)[CH2:10][C:4]=2[CH:3]=1

참가 물질

3

반응물 2

HCID 531671-MethylpiperazineHCID 12232369HCID 12232369, 화합물

생성물 1

HCID 3041883HCID 3041883, 화합물

실험 절차

12 g of 2,10-dichloro-7-fluoro-10,11-dihydro-dibenzo[b,f]thiepin are heated for 10 minutes together with 16 g of N-methylpiperazine at an external temperature of 120°-130°. After cooling the reaction mixture is poured on water and extracted with ether. The organic phase is washed with water and subsequently treated with 2 N hydrochloric acid. A precipitate is obtained. The mixture is extracted with ether, made alkaline and subsequently again extracted with ether. The organic phase is washed with water, dried over magnesium sulphate and evaporated. The so-obtained raw 1-(2-chloro-7-fluoro-10,11-dihydro-dibenzo[b,f]thiepin-10-yl)-4-methylpiperazine is converted to the corresponding maleate by treatment with maleic acid. The maleat melts at 200° with decomposition.

후처리

  1. temperatureAfter cooling the reaction mixture
  2. additionis poured on water
  3. extractionextracted with ether
  4. washThe organic phase is washed with water
  5. additionsubsequently treated with 2 N hydrochloric acid
  6. customA precipitate is obtained
  7. extractionThe mixture is extracted with ether
  8. extractionsubsequently again extracted with ether
  9. washThe organic phase is washed with water
  10. dry with materialdried over magnesium sulphate
  11. customevaporated

출처 및 근거

ORD 기록
ord-6464a597edb64584a82d22adb9e1724a
출처 데이터셋
uspto-grants-1976_06
특허 번호
US03966737

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