Dimethylformamide → 4-dimethylaminomethylene-3,4-dihydro-1H-benzo[b]azepine-2,5-dione

HRID 962517

反応式

HRID 962517 の反応式
[NH:1]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[C:5](=[O:12])[CH2:4][CH2:3][C:2]1=[O:13].[CH3:14][N:15]([CH3:18])[CH:16]=O>C(OCC)C>[CH3:14][N:15]([CH:18]=[C:4]1[C:5](=[O:12])[C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=2[NH:1][C:2](=[O:13])[CH2:3]1)[CH3:16]

参加物

4

反応物 2

HCID 6228DimethylformamideHCID 3693982,3,4,5-tetrahydro-1H-1-benzazepine-2,5-dione

生成物 1

HCID 669347634-dimethylaminomethylene-3,4-dihydro-1H-benzo[b]azepine-2,5-dione収率 79%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
90 °C

実験手順

A mixture of 0.250 g (1.43 mmol) of 3,4-dihydro-1H-1-benzazepine-2,5-dione and 5.5 ml (4.93 g, 41.5 mmol) of N,N-dimethylformamide, dimethylacetal is heated at 90° C. for 1.5 hour. The mixture is cooled, diluted with diethylether and filtered. The solid is washed well with diethylether and dried to give 0.26 g of tan crystals, m.p. 203°-205° C.

後処理

  1. temperatureThe mixture is cooled
  2. filtrationfiltered
  3. washThe solid is washed well with diethylether
  4. customdried

出典と根拠

ORDレコード
ord-c43eb5fa51df4a9695601af50598cc59
出典データセット
uspto-grants-1998_06
特許番号
US05760031

関連ノート

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