Hydrazine, propyl- → 2,3,3a,4,6,7-Hexahydro-3-phenyl-7-(phenylmethylene)-2-propylthiopyrano[4,3-c]pyrazole

HRID 1576015

반응식

HRID 1576015 반응식
[C:1]1([CH:7]=[C:8]2[C:13](=O)[C:12](=[CH:15][C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[CH2:11][S:10][CH2:9]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:22]([NH:25][NH2:26])[CH2:23][CH3:24]>CO>[C:1]1([CH:7]2[N:25]([CH2:22][CH2:23][CH3:24])[N:26]=[C:13]3[C:12](=[CH:15][C:16]4[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=4)[CH2:11][S:10][CH2:9][CH:8]23)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

4

반응물 2

HCID 42007Hydrazine, propyl-HCID 336779tetrahydro-3,5-bis(phenylmethylene)-4H-thiopyran-4-one

생성물 1

HCID 539749712,3,3a,4,6,7-Hexahydro-3-phenyl-7-(phenylmethylene)-2-propylthiopyrano[4,3-c]pyrazole수율 57.5%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 5.84g of tetrahydro-3,5-bis-(phenylmethylene)-4H-thiopyran-4-one and 1.48g of n-propyl hydrazine in 100ml of methanol is heated at reflux temperature for 3 hours. Upon cooling, solids are collected and washed with methanol. Recrystallization from methanol gives 4.0g of material, melting point 111°-120°C. Two recrystallizations from acetonitrile yield 2.0g of the title compound, melting point 119.5°-122°C.

후처리

  1. temperatureis heated
  2. temperatureat reflux temperature for 3 hours
  3. temperatureUpon cooling
  4. customsolids are collected
  5. washwashed with methanol
  6. customRecrystallization from methanol

출처 및 근거

ORD 기록
ord-d7486b977a2c4d8a9645820d2dc0b725
출처 데이터셋
uspto-grants-1976_09
특허 번호
US03979381

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