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

HRID 1605908
ノート
印刷プレビュー

反応式

HRID 1605908 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-7659c979b1de4cafb4fac39d309ea425
出典データセット
uspto-grants-1976_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03951981

反応ノート

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