Hydrochloric Acid → 6-Dicyanomethyl-1,3-dimethyluracil

HRID 648889ノート

反応式

HRID 648889 の反応式
[C:1](#[N:5])[CH2:2][C:3]#[N:4].[H-].[Na+].Cl[C:9]1[N:14]([CH3:15])[C:13](=[O:16])[N:12]([CH3:17])[C:11](=[O:18])[CH:10]=1.Cl>O1CCCC1.O>[C:3]([CH:2]([C:1]#[N:5])[C:9]1[N:14]([CH3:15])[C:13](=[O:16])[N:12]([CH3:17])[C:11](=[O:18])[CH:10]=1)#[N:4]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 8010MalononitrileHCID 24758Sodium hydrideHCID 814426-Chloro-1,3-dimethyl-2,4(1H,3H)-pyrimidinedione

生成物 1

HCID 136847646-Dicyanomethyl-1,3-dimethyluracil収率 63.2%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 6.6 g (0.1 mol) of malononitrile in 100 ml of tetrahydrofuran was added 4.0 g (0.1 mol) of 60 wt% sodium hydride under ice-cooling. Seventeen grams (0.1 mol) of 6-chloro-1,3-dimethyluracil were added thereto, followed by stirring at room temperature for 5 hours. A hundred milliliters of water were added to the mixture, and the mixture was neutralized with concentrated hydrochloric acid, followed by extraction with 200 ml of ethyl acetate. The extract was dried over anhydrous sodium sulfate, and the solvent was removed by distillation under reduced pressure, followed by filtration to obtain 12.9 g (63%) of 6-dicyanomethyl-1,3-dimethyluracil.

後処理

  1. temperaturecooling
  2. extractionfollowed by extraction with 200 ml of ethyl acetate
  3. dry with materialThe extract was dried over anhydrous sodium sulfate
  4. customthe solvent was removed by distillation under reduced pressure
  5. filtrationfollowed by filtration

出典と根拠

ORDレコード
ord-c625dde784e8470fa98570c0a6a3f616
出典データセット
uspto-grants-1988_04
特許番号
US04737442

反応ノート

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