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

HRID 355856

반응식

HRID 355856 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
90 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-38c2e7cb532c46dea5a8d0e551bd2626
출처 데이터셋
uspto-grants-1998_11
특허 번호
US05834461

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