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Potassium Iodide → 9-[4-chloro-3-(trifluoromethyl)benzyl]-4,9-dihydro-10H-thieno[3,4-b][1,5]benzodiazepin-10-one

HRID 1863188
ノート
印刷プレビュー

反応式

HRID 1863188 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+].[Cl:18][C:19]1[CH:26]=[CH:25][C:22]([CH2:23]Cl)=[CH:21][C:20]=1[C:27]([F:30])([F:29])[F:28].[I-].[K+]>CN(C)C=O>[Cl:18][C:19]1[CH:26]=[CH:25][C:22]([CH2:23][N:8]2[C:7]3[CH:12]=[CH:13][CH:14]=[CH:15][C:6]=3[NH:5][C:4]3=[CH:3][S:2][CH:1]=[C:10]3[C:9]2=[O:11])=[CH:21][C:20]=1[C:27]([F:28])([F:29])[F:30]
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 24758Sodium hydrideHCID 125216414,9-dihydro-10H-thieno[3,4-b][1,5]benzodiazepin-10-oneHCID 130942621-Chloro-4-(chloromethyl)-2-(trifluoromethyl)benzene

生成物 1

HCID 203922589-[4-chloro-3-(trifluoromethyl)benzyl]-4,9-dihydro-10H-thieno[3,4-b][1,5]benzodiazepin-10-one

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

To a solution of 8.64 g. of 4,9-dihydro-10H-thieno[3,4-b][1,5]benzodiazepin-10-one in 100 ml. of dimethylformamide is added 2.1 g. of 50% sodium hydride in mineral oil. The mixture is stirred for one hour and 10.0 g. of 4-chloro-3-trifluoromethyl benzyl chloride and 10 mg of potassium iodide are added. The mixture is stirred for a prolonged period and the solvent is removed in vacuo. The residual gum is dissolved in methylene chloride, dried over magnesium sulfate and filtered through magnesol. The filtrate is evaporated to give tan crystals which are recrystallized from ethanol giving the desired product as off-white crystals, mp. 181°-183° C.

後処理

  1. stirringThe mixture is stirred for a prolonged period
  2. customthe solvent is removed in vacuo
  3. dissolutionThe residual gum is dissolved in methylene chloride
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered through magnesol
  6. customThe filtrate is evaporated
  7. customto give tan crystals which
  8. customare recrystallized from ethanol giving the desired product as off-white crystals, mp. 181°-183° C.

出典と根拠

ORDレコード
ord-4b9804bd98b641c691ff56b341ba740a
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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