Water → 3-[5-(o-fluorophenyl)-2,3-dihydro-1,3,3-trimethyl-2-oxo-1H-1,4-benzodiazepin-7-yl]-5,5-dimethylhydantoin

HRID 354761ノート

反応式

HRID 354761 の反応式
[NH2:1][C:2]([CH3:29])([CH3:28])[C:3]([NH:5][C:6]1[CH:7]=[CH:8][C:9]2[N:15]([CH3:16])[C:14](=[O:17])[C:13]([CH3:19])([CH3:18])[N:12]=[C:11]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=3[F:26])[C:10]=2[CH:27]=1)=[O:4].[C:30](Cl)(Cl)=[O:31].C(N(CC)CC)C.O>ClCCCl>[F:26][C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=1[C:11]1[C:10]2[CH:27]=[C:6]([N:5]3[C:3](=[O:4])[C:2]([CH3:29])([CH3:28])[NH:1][C:30]3=[O:31])[CH:7]=[CH:8][C:9]=2[N:15]([CH3:16])[C:14](=[O:17])[C:13]([CH3:19])([CH3:18])[N:12]=1

参加物

6

反応物 4

HCID 962WaterHCID 6371PhosgeneHCID 8471TriethylamineHCID 20506149HCID 20506149、化合物

生成物 1

HCID 205061833-[5-(o-fluorophenyl)-2,3-dihydro-1,3,3-trimethyl-2-oxo-1H-1,4-benzodiazepin-7-yl]-5,5-dimethylhydantoin

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒2 回

実験手順

2 g (0.005 mol) of 2 amino-N-[5-(o-fluorophenyl)-2,3-dihydro-1,3,3-trimethyl-2-oxo-1H-1,4-benzodiazepin-7-yl]-2-methylpropionamide are dissolved in 50 ml of 1,2-dichloroethane and added to 1 g of phosgene in 50 ml of 1,2-dichloroethane at room temperature. The reaction mixture is stirred for 1/2 hour and subsequently made basic with triethylamine. The mixture is treated with water and extracted with methylene chloride. The organic phase is dried and evaporated. The residue gives, from ethyl acetate/ether, 3-[5-(o-fluorophenyl)-2,3-dihydro-1,3,3-trimethyl-2-oxo-1H-1,4-benzodiazepin-7-yl]-5,5-dimethylhydantoin of melting point 286°-287°.

後処理

  1. extractionextracted with methylene chloride
  2. customThe organic phase is dried
  3. customevaporated

出典と根拠

ORDレコード
ord-60969652dcb94f80a05a96160cfbba6f
出典データセット
uspto-grants-1983_03
特許番号
US04377522

反応ノート

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