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

HRID 647954ノート

反応式

HRID 647954 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

反応条件

温度
190 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-435995b547684be592cbb36143f2d1d8
出典データセット
uspto-grants-1983_10
特許番号
US04410536

反応ノート

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