Water → 1-Ethyl-7-methoxy-5-methyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione

HRID 1504210ノート

反応式

HRID 1504210 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[NH:12][C:11](=[O:13])[CH2:10][C:9](=[O:14])[N:8]([CH3:15])[C:7]=2[CH:16]=1.[CH2:17](I)[CH3:18].O>C(OCC)(=O)C>[CH2:17]([N:12]1[C:11](=[O:13])[CH2:10][C:9](=[O:14])[N:8]([CH3:15])[C:7]2[CH:16]=[C:3]([O:2][CH3:1])[CH:4]=[CH:5][C:6]1=2)[CH3:18]

参加物

5

反応物 3

HCID 962WaterHCID 6340IodoethaneHCID 669610818-Methoxy-1-methyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione

生成物 1

HCID 686748151-Ethyl-7-methoxy-5-methyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione収率 76.7%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
0 °C

実験手順

8-Methoxy-1-methyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione (220 mg) was added to the suspension at the same temperature, and stirred at 0° C. for 1 hour. Ethyl iodide (187 mg) was added to the mixture and stirred at room temperature overnight. Water was added to the reaction mixture, and extraction with ethyl acetate was performed. The organic layer was dried over sodium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=4:1→1:1). The purified product was concentrated to dryness under reduced pressure to give the title compound(190.2 mg) as a yellow solid.

後処理

  1. stirringstirred at room temperature overnight
  2. dry with materialThe organic layer was dried over sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=4:1→1:1)
  5. concentrationThe purified product was concentrated to dryness under reduced pressure

出典と根拠

ORDレコード
ord-f1cb18a2488a4c4d980def2d8d83569e
出典データセット
uspto-grants-2015_12
特許番号
US09212187B2

反応ノート

読み込み中…