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

HRID 1605911ノート

反応式

HRID 1605911 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 176Acetic Acid触媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-7496b1d359354a71bff7bc6b4219eba1
出典データセット
uspto-grants-1976_04
特許番号
US03951981

反応ノート

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