1-Methylpiperazine → 4H-Thieno(3,4-b)(1,5)benzodiazepine, 7-chloro-10-(4-methyl-1-piperazinyl)-

HRID 1605911노트

반응식

HRID 1605911 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][C:10]3=[CH:12][S:13][CH:14]=[C:9]3[C:8](SC)=[N:7][C:6]=2[CH:17]=1.[CH3:18][N:19]1[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1>C(O)(=O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][C:10]3=[CH:12][S:13][CH:14]=[C:9]3[C:8]([N:22]3[CH2:23][CH2:24][N:19]([CH3:18])[CH2:20][CH2:21]3)=[N:7][C:6]=2[CH:17]=1

참가 물질

4

반응물 2

HCID 531671-MethylpiperazineHCID 125216627-Chloro-10-(methylthio)-4H-thieno[3,4-b] [1,5]benzodiazepine

생성물 1

HCID 30423894H-Thieno(3,4-b)(1,5)benzodiazepine, 7-chloro-10-(4-methyl-1-piperazinyl)-

시약·촉매·용매 1

HCID 176Acetic Acid촉매

실험 절차

A solution of 0.9 g. of 7-chloro-10-(methylthio)-4H-thieno[3,4-b] [1,5] benzodiazepine in 4.5 ml. of N-methylpiperazine is treated with 2-3 drops of glacial acetic acid and heated under reflux for 4 days. The solution is concentrated to dryness and the residue is warmed with dilute acetic acid. The acidic solution is filtered, cooled and made alkaline with concentrated ammonium hydroxide. The sticky precipitate is collected and dissolved in chloroform. The dried chloroform solution is concentrated under reduced pressure to give 7-chloro-10-(4-methyl-1-piperazinyl)-4H-thieno[3,4-b] [1,5] benzodiazepine as an oil. An ethanolic solution of the oil is treated with 70% perchloric acid and diluted with water. The precipitate is recrystallized from methanol to give yellow crystals, m.p. 268°-270°C. (dec.).

후처리

  1. temperatureheated
  2. temperatureunder reflux for 4 days
  3. concentrationThe solution is concentrated to dryness
  4. temperaturethe residue is warmed with dilute acetic acid
  5. filtrationThe acidic solution is filtered
  6. temperaturecooled
  7. customThe sticky precipitate is collected
  8. dissolutiondissolved in chloroform
  9. concentrationThe dried chloroform solution is concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-7496b1d359354a71bff7bc6b4219eba1
출처 데이터셋
uspto-grants-1976_04
특허 번호
US03951981

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