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Piperidine → HCID 20355332, 화합물

HRID 1605906
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HRID 1605906 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][CH2:20][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][CH2:20][CH2:19][CH2:18]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 8082PiperidineHCID 12521659HCID 12521659, 화합물

생성물 1

HCID 20355332HCID 20355332, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A solution of 0.7 g. of 10-(methylthio)-4H-thieno[3,4-b] [1,5] benzodiazepine in 5 ml. of piperidine is treated with a drop of glacial acetic acid and heated under reflux for 4 days. Excess piperidine is removed under reduce pressure and the oily residue is warmed with dilute acetic acid and filtered. The filtrate is cooled and made alkaline with concentrated ammonium hydroxide to give a yellow solid. Recrystallization from acetone-petroleum ether (30°-60°C.) gives yellow crystals, m.p. 157°-159°C.

후처리

  • temperatureheated
  • temperatureunder reflux for 4 days
  • customExcess piperidine is removed
  • temperaturethe oily residue is warmed with dilute acetic acid
  • filtrationfiltered
  • temperatureThe filtrate is cooled
  • customto give a yellow solid
  • customRecrystallization from acetone-petroleum ether (30°-60°C.)
  • customgives yellow crystals, m.p. 157°-159°C.
  • 출처 및 근거

    ORD 기록
    ord-cdcd9543f68746ed8f5f199c26087641
    출처 데이터셋
    uspto-grants-1976_04
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US03951981

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