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Methyl iodide → 5-(o-fluorophenyl)-1,3-dihydro-1,3,3-trimethyl-7-nitro-2H-1,4-benzodiazepin-2-one

HRID 354738
ノート
印刷プレビュー

反応式

HRID 354738 の反応式
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:14]2[CH:15]=[C:16]([N+:19]([O-:21])=[O:20])[CH:17]=[CH:18][C:13]=2[NH:12][C:11](=[O:22])[C:10]([CH3:24])([CH3:23])[N:9]=1.[C:25](=O)([O-])[O-].[K+].[K+].CI>CC(C)=O>[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:14]2[CH:15]=[C:16]([N+:19]([O-:21])=[O:20])[CH:17]=[CH:18][C:13]=2[N:12]([CH3:25])[C:11](=[O:22])[C:10]([CH3:24])([CH3:23])[N:9]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 205061515-(o-fluorophenyl)-1,3-dihydro-3,3-dimethyl-7-nitro-2H-1,4-benzodiazepin-2-one

生成物 1

HCID 205061565-(o-fluorophenyl)-1,3-dihydro-1,3,3-trimethyl-7-nitro-2H-1,4-benzodiazepin-2-one

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

18.2 g (0.056 mol) of 5-(o-fluorophenyl)-1,3-dihydro-3,3-dimethyl-7-nitro-2H-1,4-benzodiazepin-2-one are dissolved in 150 ml of dry acetone, treated with 18 g of powdered potassium carbonate and 9 ml of methyl iodide and stirred at room temperature for 21/2 hours. Subsequently, the reaction mixture is evaporated and the residue is partitioned between methylene chloride and water. After separating the organic phase, it is extracted several times more with methylene chloride. The combined organic extracts are then dried and evaporated. The residue is recrystallized from benzene/hexane/petroleum ether and gives 5-(o-fluorphenyl)-1,3-dihydro-1,3,3-trimethyl-7-nitro-2H-1,4-benzodiazepin-2-one of melting point 128°-129°.

後処理

  1. customSubsequently, the reaction mixture is evaporated
  2. customthe residue is partitioned between methylene chloride and water
  3. customAfter separating the organic phase, it
  4. extractionis extracted several times more with methylene chloride
  5. customThe combined organic extracts are then dried
  6. customevaporated
  7. customThe residue is recrystallized from benzene/hexane/petroleum ether

出典と根拠

ORDレコード
ord-3def78dc81f44728989a2ea9c7f0b1f9
出典データセット
uspto-grants-1983_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04377522

反応ノート

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