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1-Ethylpiperazine → HCID 12521672, 화합물

HRID 371650
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HRID 371650 반응식
CS[C:3]1[C:4]2[C:5](=[CH:14][S:15][CH:16]=2)[NH:6][C:7]2[CH:13]=[CH:12][CH:11]=[CH:10][C:8]=2[N:9]=1.[CH2:17]([N:19]1[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1)[CH3:18]>C(O)(=O)C>[CH2:17]([N:19]1[CH2:24][CH2:23][N:22]([C:3]2[C:4]3[C:5](=[CH:14][S:15][CH:16]=3)[NH:6][C:7]3[CH:13]=[CH:12][CH:11]=[CH:10][C:8]=3[N:9]=2)[CH2:21][CH2:20]1)[CH3:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 791961-EthylpiperazineHCID 12521659HCID 12521659, 화합물

생성물 1

HCID 12521672HCID 12521672, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid촉매

실험 절차

A mixture comprising 2.5 g. of 10-(methylthio)-4H-thieno[3,4-b][1,5]benzodiazepine (U.S. Pat. No. 3,951,981 -- Ex. 2), 11.4 g. of N-ethylpiperazine and 3 drops of acetic acid is stirred and refluxed overnight. The mixture is evaporated. The residue is slurried in water and then the residue is dissolved in 50 ml. of 2N acetic acid, filtered and the filtrate is made alkaline with ammonium hydroxide. The mixture is cooled and filtered. The solid is recrystallized twice from ethanol giving 10-(4-ethyl-1-piperazinyl)-4H-thieno[3,4-b][1,5]benzodiazepine.

후처리

  1. temperaturerefluxed overnight
  2. customThe mixture is evaporated
  3. dissolutionthe residue is dissolved in 50 ml
  4. filtrationof 2N acetic acid, filtered
  5. temperatureThe mixture is cooled
  6. filtrationfiltered
  7. customThe solid is recrystallized twice from ethanol

출처 및 근거

ORD 기록
ord-7c6fbaafc1db4d03896a02abeb3b51ce
출처 데이터셋
uspto-grants-1978_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04087421

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