3-(1-Piperazinyl)propanamide → HCID 128684, 화합물

HRID 2118483노트

반응식

HRID 2118483 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.[N:19]1([CH2:25][CH2:26][C:27]([NH2:29])=[O:28])[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1>C(Cl)(Cl)Cl>[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:22]3[CH2:21][CH2:20][N:19]([CH2:25][CH2:26][C:27]([NH2:29])=[O:28])[CH2:24][CH2:23]3)[CH2:10][C:4]=2[CH:3]=1

참가 물질

4

반응물 2

HCID 5446973-(1-Piperazinyl)propanamideHCID 12232369HCID 12232369, 화합물

생성물 1

HCID 128684HCID 128684, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

A mixture of 2,10-dichloro-7-fluoro-10,11-dihydrodibenzo(b,f)-thiepin (2.8 g), 3-(1-piperazinyl)propionamide (3.2 g) and chloroform (10 ml) is refluxed with stirring for 8 hours. The solvent is than evaporated under reduced pressure, and the residue is extracted by shaking with a two-phase system consisting of benzene (30 ml) and a solution of methanesulfonic acid (4 g) in water (50 ml). The clear aqueous solution is separated and then made alkaline with aqueous ammonia (10 ml). The so-formed suspension of the amorphous base is diluted with ethanol (100 ml), and the mixture is briefly warmed to boiling. The resultant clear solution is then allowed to crystallize at room temperature for 6 hours. The crystalline product is separated, washed with a small amount of ethanol, and then dried in vacuo. The obtained base (2.35 g, 60% of theory) melts at 179°-182° C.; it can be purified by crystallization from ethanol to give the title compound having a m.p. of 182°-184° C. and which is identical with the product of the preceding example 1.

후처리

  1. temperatureis refluxed
  2. customthan evaporated under reduced pressure
  3. extractionthe residue is extracted
  4. stirringby shaking with a two-phase system
  5. customThe clear aqueous solution is separated
  6. additionThe so-formed suspension of the amorphous base
  7. additionis diluted with ethanol (100 ml)
  8. temperaturethe mixture is briefly warmed to boiling
  9. customto crystallize at room temperature for 6 hours
  10. customThe crystalline product is separated
  11. washwashed with a small amount of ethanol
  12. customdried in vacuo
  13. customit can be purified by crystallization from ethanol

출처 및 근거

ORD 기록
ord-f1715414a7be4906bdb636d7589ad38c
출처 데이터셋
uspto-grants-1987_07
특허 번호
US04678788

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