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

HRID 542707ノート

反応式

HRID 542707 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>O.O1CCCC1>[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

Then, to a solution comprising of 100 ml of a tetrahydrofuran and 6.6 g (0.1 mole) of malononitrile was added 4.0 g (0.1 mole) of 60 wt% sodium hydride in nujol (paraffin oil) under ice-cooling, and, after adding thereto 17 g (0.1 mole) of 6-chloro-1,3-dimethyluracil, the mixture was stirred for 5 hours at room temperature. The reaction mixture thus obtained was mixed with 100 ml of water, neutralized with concentrated hydrochloric acid, and thereafter extracted with 200 ml of ethyl acetate. The extract was dried by anhydrous sodium sulfate, the solvent was distilled off under reduced pressure, and the crystals thus precipitated were collected by filtration to provide 12.9 g (63%) of 6-dicyanomethyl-1,3-dimethyluracil.

後処理

  1. temperaturecooling
  2. additionafter adding
  3. customThe reaction mixture thus obtained
  4. extractionextracted with 200 ml of ethyl acetate
  5. dry with materialThe extract was dried by anhydrous sodium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. customthe crystals thus precipitated
  8. filtrationwere collected by filtration

出典と根拠

ORDレコード
ord-28b45f4e492846c1822da21365f68ddc
出典データセット
uspto-grants-1987_04
特許番号
US04659651

反応ノート

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