Water → 1-Ethyl-7-hydroxy-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione

HRID 1504211ノート

反応式

HRID 1504211 の反応式
B(Br)(Br)Br.ClCCl.[CH2:8]([N:10]1[C:16](=[O:17])[C:15]([CH3:19])([CH3:18])[C:14](=[O:20])[N:13]([CH3:21])[C:12]2[CH:22]=[C:23]([O:26]C)[CH:24]=[CH:25][C:11]1=2)[CH3:9].O>CO.ClCCl>[CH2:8]([N:10]1[C:16](=[O:17])[C:15]([CH3:19])([CH3:18])[C:14](=[O:20])[N:13]([CH3:21])[C:12]2[CH:22]=[C:23]([OH:26])[CH:24]=[CH:25][C:11]1=2)[CH3:9]

参加物

6

反応物 3

HCID 962WaterHCID 22277759Boron tribromide dichloromethaneHCID 686743071-Ethyl-7-methoxy-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione

生成物 1

HCID 686733851-Ethyl-7-hydroxy-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione収率 97.5%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 6344Dichloromethane溶媒2 回

実験手順

A 1.0 M boron tribromide/dichloromethane solution (1.22 ml) was added to a dichloromethane solution (3 ml) of 1-ethyl-7-methoxy-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione (169 mg) at 0° C., and stirred at room temperature overnight. Water and methanol were added to the reaction mixture and extraction with the mixture solvent (dichloromethane:methanol=10:1) was performed. The organic layer was dried over anhydrous sodium sulfate, and concentrated to dryness under reduced pressure to give the title compound(156.4 mg) as a white powder.

後処理

  1. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  2. concentrationconcentrated to dryness under reduced pressure

出典と根拠

ORDレコード
ord-a0ebfcfc0b394fc9a3eef3631081c32b
出典データセット
uspto-grants-2015_12
特許番号
US09212187B2

反応ノート

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