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

HRID 542707노트

반응식

HRID 542707 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

HCID 136847646-Dicyanomethyl-1,3-dimethyluracil수율 63.2%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-28b45f4e492846c1822da21365f68ddc
출처 데이터셋
uspto-grants-1987_04
특허 번호
US04659651

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