Ethanol → HCID 86658681, 화합물

HRID 42691

반응식

HRID 42691 반응식
[Na].Cl[C:3]1[N:8]([CH3:9])[C:7](=[O:10])[N:6]([CH3:11])[C:5](=[O:12])[C:4]=1[CH:13]=[O:14].[CH2:15]([OH:17])[CH3:16]>>[CH2:15]([O:17][C:3]1[N:8]([CH3:9])[C:7](=[O:10])[N:6]([CH3:11])[C:5](=[O:12])[C:4]=1[CH:13]=[O:14])[CH3:16]

참가 물질

4

반응물 3

HCID 702EthanolHCID 3199716-Chloro-5-formyl-1,3-dimethyluracilHCID 5360545Sodium

생성물 1

HCID 86658681HCID 86658681, 화합물

실험 절차

To a stirred solution of sodium (3.82 mmol) in ethanol (3.8 ml) under argon at 5-7° C., 6-chloro-1,3-dimethyl-2,4-dioxo-1,2,3,4-tetrahydropyrimidine-5-carbaldehyde (2.67 mmol) (Tetrahedron Lett., 1993, 34(51), 8213-8216) was added. The resulting mixture was stirred at room temperature under argon for 1 h. Then it was evaporated to dryness in vacuo and the residue was stirred in a mixture of ice-water (40 ml) and ethyl acetate (20 ml). After separation of the phases, the aqueous phase was extracted with ethyl acetate (20 ml). The combined organic phases were washed with water, brine and dried over anhydrous MgSO4. The solvent was evaporated in vacuo, and the crude product was purified by column chromatography with a mixture of n-hexane:ethyl acetate (1:1) as the eluent.

후처리

  1. customThen it was evaporated to dryness in vacuo
  2. stirringthe residue was stirred in a mixture of ice-water (40 ml) and ethyl acetate (20 ml)
  3. customAfter separation of the phases
  4. extractionthe aqueous phase was extracted with ethyl acetate (20 ml)
  5. washThe combined organic phases were washed with water, brine
  6. dry with materialdried over anhydrous MgSO4
  7. customThe solvent was evaporated in vacuo
  8. customthe crude product was purified by column chromatography with a mixture of n-hexane:ethyl acetate (1:1) as the eluent

출처 및 근거

ORD 기록
ord-210a3951b43e4a669c3ca1267f7ea894
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08536210B2

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