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Piperazine → 4H-Thieno(3,4-b)(1,5)benzodiazepine, 10-(1-piperazinyl)-

HRID 371629
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반응식

HRID 371629 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.[NH:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1>C(O)(=O)C>[N:17]1([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)[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 4837PiperazineHCID 12521659HCID 12521659, 화합물

생성물 1

HCID 30423884H-Thieno(3,4-b)(1,5)benzodiazepine, 10-(1-piperazinyl)-

시약·촉매·용매 2

HCID 176Acetic Acid촉매HCID 176Acetic Acid용매

실험 절차

A bomb charged with 2.5 g. of 10-(methylthio)-4H-thieno[3,4-b][1,5]benzodiazepine, 8.6 g. of piperazine, and three drops of acetic acid is placed in an oil bath and heated at 155°-160° C. for 4 days. The bomb is then cooled and the contents are dissolved in 2N acetic acid. The solution is filtered and the filtrate is made alkaline with ammonium hydroxide and extracted with chloroform. The extracts are dried, filtered and evaporated to give a yellow solid. Recrystallization from ethanol gives the product as light tan crystals which melt at 228°-231° C. (dec.).

후처리

  1. additionA bomb charged with 2.5 g
  2. temperatureheated at 155°-160° C. for 4 days
  3. temperatureThe bomb is then cooled
  4. filtrationThe solution is filtered
  5. extractionextracted with chloroform
  6. customThe extracts are dried
  7. filtrationfiltered
  8. customevaporated
  9. customto give a yellow solid
  10. customRecrystallization from ethanol

출처 및 근거

ORD 기록
ord-cc6f6cc5ab9c4ef6986daf09cce11c4c
출처 데이터셋
uspto-grants-1978_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04087421

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