Methanol → HCID 178426048、化合物

反応式

[F:1][C:2]([F:10])([F:9])[C:3](=O)[CH2:4][C:5](=O)[CH3:6].[C:11](#[N:15])[CH2:12][C:13]#[N:14].C[OH:17]>>[OH:17][C:11]1[N:15]=[C:5]([CH3:6])[CH:4]=[C:3]([C:2]([F:10])([F:9])[F:1])[C:12]=1[C:13]#[N:14]

参加物

反応物 3

HCID 887Methanol

HCID 8010Malononitrile

HCID 739431,1,1-Trifluoro-2,4-pentanedione

生成物 1

HCID 178426048HCID 178426048、化合物収率 40%

実験手順

To a solution of 1,1,1-trifluoropentane-2,4-dione (5.8 g, 37.7 mmol) in methanol (20 mL) was added malononitrile (5 g, 75 mmol) and then the mixture was heated to reflux. The mixture was maintained at the same temperature for 12 hours. The resultant mixture was cooled to room temperature, and then filtered. The solid was washed with methanol to give pure 2-hydroxy-6-methyl-4-(trifluoromethyl)nicotinonitrile (3 g, 40%). 1H NMR (300 MHz, d6-DMSO): δ 13.36 (s, 1H), 6.65 (s, 1H), 2.38 (s, 3H).