ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Potassium Hydroxide → 4-Methyl-10-(methylthio)-4H-thieno[3,4-b] [1,5]benzodiazepine

HRID 371632
ノート
印刷プレビュー

反応式

HRID 371632 の反応式
[CH3:1][N:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[NH:6][C:5](=[S:13])[C:4]2=[CH:14][S:15][CH:16]=[C:3]12.O1CCOC[CH2:18]1.[OH-].[K+].S([O-])(OC)(=O)=O>CO>[CH3:1][N:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[N:6]=[C:5]([S:13][CH3:18])[C:4]2=[CH:14][S:15][CH:16]=[C:3]12
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 14797Potassium HydroxideHCID 312751,4-DioxaneHCID 4694097Methyl sulfate(1-)HCID 125216534,9-Dihydro-4-methyl-10H-thieno[3,4-b][1,5]benzodiazepin-10-thione

生成物 1

HCID 125216604-Methyl-10-(methylthio)-4H-thieno[3,4-b] [1,5]benzodiazepine

試薬・触媒・溶媒 1

HCID 887Methanol
溶媒
2 回

実験手順

To a stirred suspension of 0.7 g. of 4,9-dihydro-4-methyl-10H-thieno[3,4-b][1,5]benzodiazepin-10-thione in 10 ml. of dioxane is added dropwise and simultaneously at 30°-40° C., a solution of 0.95 g. of potassium hydroxide in 10 ml. of methanol and 0.8 ml. of methyl sulfate. After addition is complete the mixture is stirred for 3 hours, diluted with methanol and filtered. The filtrate is concentrated to about 20 ml., diluted with water and extracted with chloroform. The chloroform solution is concentrated to give a solid, which is recrystallized from methanol-water to give orgnae crystals, m.p. 113°-115° C.

後処理

  1. additionTo a stirred suspension of 0.7 g
  2. additionAfter addition
  3. filtrationfiltered
  4. concentrationThe filtrate is concentrated to about 20 ml
  5. addition, diluted with water
  6. extractionextracted with chloroform
  7. concentrationThe chloroform solution is concentrated
  8. customto give a solid, which
  9. customis recrystallized from methanol-water
  10. customto give orgnae crystals, m.p. 113°-115° C.

出典と根拠

ORDレコード
ord-a203c0e1bfd248a796c91774b6b49d03
出典データセット
uspto-grants-1978_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04087421

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート