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Potassium Iodide → 4,9-Dihydro-9-phenethyl-10H-thieno[3,4-b][1,5]benzodiazepin-10-one

HRID 1863187
ノート
印刷プレビュー

反応式

HRID 1863187 の反応式
[CH:1]1[S:2][CH:3]=[C:4]2[C:10]=1[C:9](=[O:11])[NH:8][C:7]1[CH:12]=[CH:13][CH:14]=[CH:15][C:6]=1[NH:5]2.[H-].[Na+].[CH2:18](Br)[CH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1.[I-].[K+]>CN(C)C=O>[CH2:18]([N:8]1[C:7]2[CH:12]=[CH:13][CH:14]=[CH:15][C:6]=2[NH:5][C:4]2=[CH:3][S:2][CH:1]=[C:10]2[C:9]1=[O:11])[CH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1
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 4875Potassium IodideHCID 7666Phenethyl bromideHCID 24758Sodium hydrideHCID 125216414,9-dihydro-10H-thieno[3,4-b][1,5]benzodiazepin-10-one

生成物 1

HCID 203922654,9-Dihydro-9-phenethyl-10H-thieno[3,4-b][1,5]benzodiazepin-10-one

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide
溶媒

実験手順

To a solution of 17.28 g. of 4,9-dihydro-10H-thieno[3,4-b][1,5]benzodiazepin-10-one in 100 ml. of dimethylformamide is added 4.2 g. of 50% sodium hydride in mineral oil. The mixture is stirred for one hour and 16.0 g. of phenethyl bromide and 20 mg. of potassium iodide are added. The mixture is stirred for 48 hours. The solution is evaporated. The residual gum is washed with water and hexane, dissolved in methylene chloride, washed with water, dried over magnesium sulfate and filtered through magnesol. The crystals which form in the filtrate are removed by filtration. This filtrate is evaporated in vacuo giving the desired product as dark brown crystals.

後処理

  1. stirringThe mixture is stirred for 48 hours
  2. customThe solution is evaporated
  3. washThe residual gum is washed with water and hexane
  4. dissolutiondissolved in methylene chloride
  5. washwashed with water
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered through magnesol
  8. customThe crystals which form in the filtrate
  9. customare removed by filtration
  10. customThis filtrate is evaporated in vacuo

出典と根拠

ORDレコード
ord-1160cc3d332e476a916e5b7f67887aab
出典データセット
uspto-grants-1979_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04168269

反応ノート

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