Ethyl Acetate → HCID 10403166、化合物

HRID 1755630ノート

反応式

HRID 1755630 の反応式
[Br:1]Br.[C:3]([N:7]1[C:13](=[O:14])[C:12]2[CH:15]=[CH:16][CH:17]=[CH:18][C:11]=2[NH:10][C:9](=[O:19])[CH2:8]1)([CH3:6])([CH3:5])[CH3:4].C([O-])(=O)C.[Na+].C(OCC)(=O)C>C(O)(=O)C>[Br:1][C:16]1[CH:17]=[CH:18][C:11]2[NH:10][C:9](=[O:19])[CH2:8][N:7]([C:3]([CH3:6])([CH3:4])[CH3:5])[C:13](=[O:14])[C:12]=2[CH:15]=1

参加物

6

反応物 4

HCID 8857Ethyl AcetateHCID 24408BromineHCID 517045Sodium AcetateHCID 100826661H-1,4-Benzodiazepine-2,5-dione, 4-(1,1-dimethylethyl)-3,4-dihydro-

生成物 1

HCID 10403166HCID 10403166、化合物収率 64.3%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

Bromine (1.72 g, 10.8 mmol) is added to a mixture of 4-tert-butyl-3,4-dihydro-1H-1,4-benzodiazepine-2,5-dione (1.0 g, 4.3 mmol) and sodium acetate (0.39 g, 4.8 mmol) in acetic acid. The reaction mixture is stirred at room temperature for 29 hours, concentrated in vacuo, diluted with ethyl acetate, washed sequentially with 0.1N sodium hydroxide solution and brine, dried over anhydrous sodium sulfate and concentrated in vacuo to give a residue. Chromatography of the residue using silica gel and 20% to 25% ethyl acetate in hexanes solutions gives the title product as a white solid (0.86 g, mp 205°-208° C.).

後処理

  1. concentrationconcentrated in vacuo
  2. additiondiluted with ethyl acetate
  3. washwashed sequentially with 0.1N sodium hydroxide solution and brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customto give a residue

出典と根拠

ORDレコード
ord-dab398a0f9f7430081f72a7e6c45e221
出典データセット
uspto-grants-1995_08
特許番号
US05438035

反応ノート

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