N-Phenethyl-4-piperidinone → 9-Phenethyl-1-phenyl-7,8,9,10-tetrahydrothieno[3,2-e]pyrido[4,3-b]indole

HRID 647954노트

반응식

HRID 647954 반응식
Cl.[NH:2]([C:4]1[CH:5]=[CH:6][C:7]2[S:11][CH:10]=[C:9]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[C:8]=2[CH:18]=1)N.[CH2:19]1[C:24](=O)[CH2:23][CH2:22][N:21]([CH2:26][CH2:27][C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)[CH2:20]1>C(O)(C)C>[CH2:26]([N:21]1[CH2:22][CH2:23][C:24]2[NH:2][C:4]3[C:18]([C:19]=2[CH2:20]1)=[C:8]1[C:9]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[CH:10][S:11][C:7]1=[CH:6][CH:5]=3)[CH2:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1

참가 물질

4

반응물 2

HCID 96437N-Phenethyl-4-piperidinoneHCID 204842955-Hydrazino-3-phenylbenzothiophene hydrochloride

생성물 1

HCID 204843199-Phenethyl-1-phenyl-7,8,9,10-tetrahydrothieno[3,2-e]pyrido[4,3-b]indole

시약·촉매·용매 1

HCID 3776Isopropanol용매

반응 조건

온도
190 °C

실험 절차

28.0 g of 5-hydrazino-3-phenylbenzothiophene hydrochloride are allowed to react with 21.0 g of N-(2-phenethyl)-4-piperidone in 500 ml of isopropanol at room temperature for 2 hours. After filtering off the crystall sludge, this is suspended in 150 ml of N NaOH and the suspension is extracted with methylene chloride. The organic phase is washed with water until neutral and evaporated, the oily residue is taken up in 400 ml of ethylene glycol and the mixture is heated to 190° C. for 30 minutes. The substance which has crystallised out after cooling is filtered off and recrystallised from toluene. Melting point: 220°-221° C.

후처리

  1. filtrationAfter filtering off the crystall sludge
  2. extractionthe suspension is extracted with methylene chloride
  3. washThe organic phase is washed with water until neutral and
  4. customevaporated
  5. customThe substance which has crystallised out
  6. temperatureafter cooling
  7. filtrationis filtered off
  8. customrecrystallised from toluene

출처 및 근거

ORD 기록
ord-435995b547684be592cbb36143f2d1d8
출처 데이터셋
uspto-grants-1983_10
특허 번호
US04410536

반응 노트

불러오는 중…