Trifluoroacetic acid → 5-(3-Methoxy-allylidene)-1,3-dimethyl-pyrimidine-2,4,6-trione

HRID 76821

反応式

HRID 76821 の反応式
[CH3:1][N:2]1[C:9](=[O:10])[CH2:8][C:6](=[O:7])[N:5]([CH3:11])[C:3]1=[O:4].[CH3:12][O:13][CH:14](OC)[CH2:15][CH:16](OC)OC.FC(F)(F)C(O)=O>>[CH3:12][O:13][CH:14]=[CH:15][CH:16]=[C:8]1[C:9](=[O:10])[N:2]([CH3:1])[C:3](=[O:4])[N:5]([CH3:11])[C:6]1=[O:7]

参加物

4

反応物 3

HCID 6422Trifluoroacetic acidHCID 66019TetramethoxypropaneHCID 69860Dimethylbarbituric acid

生成物 1

HCID 766881855-(3-Methoxy-allylidene)-1,3-dimethyl-pyrimidine-2,4,6-trione

反応条件

温度
100 °C

実験手順

1,3-Dimethylbarbituric acid (20 g, 0.1 mol; Aldrich) was placed in 100 mL round-bottom one-necked flask equipped with magnetic stir bar and reflux condenser, 1,1,3,3-tetramethoxy-propane, (40 mL, 0.2 mol; Aldrich) and 1 mL of Trifluoroacetic Acid (2 mL, 0.03 mol; Sigma) were added to the reaction mixture. The flask was heated at 100° C. with stirring for 5 hours and then cooled to room temperature. The crystallized product was filtered, washed with methanol and dried. The yield was 23 g (80% of theory).

後処理

  1. customequipped with magnetic stir bar
  2. temperaturereflux condenser
  3. temperaturecooled to room temperature
  4. filtrationThe crystallized product was filtered
  5. washwashed with methanol
  6. customdried

出典と根拠

ORDレコード
ord-083eb0ef8a61487aa5f4542b7ed912c4
出典データセット
uspto-grants-2014_09
特許番号
US08835632B2

関連ノート

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