Dimethylformamide dimethyl acetal → HCID 59436236、化合物

HRID 1805460ノート

反応式

HRID 1805460 の反応式
[F:1][CH:2]([F:22])[O:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[NH:10][N:11]=[C:12]([C:17](=[O:21])[CH2:18][O:19][CH3:20])[C:13]([O:15][CH3:16])=[O:14].[CH3:23]OC(OC)N(C)C>>[F:1][CH:2]([F:22])[O:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[N:10]1[CH:23]=[C:18]([O:19][CH3:20])[C:17](=[O:21])[C:12]([C:13]([O:15][CH3:16])=[O:14])=[N:11]1

参加物

3

反応物 2

HCID 78373Dimethylformamide dimethyl acetalHCID 178496276HCID 178496276、化合物

生成物 1

HCID 59436236HCID 59436236、化合物収率 88%

実験手順

A solution of methyl 2-{[2-(difluoromethoxy)phenyl]hydrazono}-4-methoxy-3-oxobutanoate (8.70 g, 27.5 mmol) in N,N-dimethylformamide dimethyl acetal (60 mL) was refluxed for 3 h and stirred at room temperature for 3 days. The precipitate was collected by filtration and washed with hexane/AcOEt (3/1) to give the title compound (7.92 g, 88% yield) as yellow crystals: 1H NMR (300 MHz, CDCl3): δ ppm 3.89 (3H, s), 3.96 (3H, s), 6.55 (1H, d, J=72.7 Hz), 7.35-7.45 (2H, m), 7.49-7.56 (1H, m), 7.61 (1H, dd, J=7.9, 1.5 Hz), 7.73 (1H, s).

後処理

  1. filtrationThe precipitate was collected by filtration
  2. washwashed with hexane/AcOEt (3/1)

出典と根拠

ORDレコード
ord-c3a2c390de1e4da3a53806f6c11b59ba
出典データセット
uspto-grants-2013_01
特許番号
US08354411B2

反応ノート

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