Water → HCID 15059441, 화합물

HRID 35817노트

반응식

HRID 35817 반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[N:6]=[C:5]([C:11]([CH:22]([CH3:24])[CH3:23])(C(OCC)=O)[C:12]([O:14]CC)=[O:13])[N:4]=1.[OH-].[Na+].O>CO>[CH3:10][O:9][C:7]1[CH:8]=[C:3]([O:2][CH3:1])[N:4]=[C:5]([CH:11]([CH:22]([CH3:24])[CH3:23])[C:12]([OH:14])=[O:13])[N:6]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 15239781Diethyl 2-(4,6-dimethoxypyrimidin-2-yl)-2-isopropylmalonate

생성물 1

HCID 15059441HCID 15059441, 화합물수율 75.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

10 g of diethyl 2-(4,6-dimethoxypyrimidin-2-yl)-2-isopropylmalonate, 5,0 g of sodium hydroxide, 20 ml of water and 50 ml of methanol were placed in a round bottom flask, and were stirred under heat-refluxing for 6 hours. The reaction liquor was concentrated, and 100 ml of water was added thereto. The reaction liquor was adjusted to a pH of from 3 to 4 with a dilute hydrochloric acid under cooling with ice, and was extracted twice with 100 ml of diethyl ether. The extracted liquor was washed with water, and was dried with anhydrous sodium sulfate for one night. After filtrating the inorganic salt, the solvent was distilled off under reduced pressure to obtain 5.8 g of a crude crystal. The crude crystal thus obtained was recrystallized from ether-hexane to obtain 5.3 g of the aimed product of white powder (yield=75.1%) having a melting point of 99°-101° C.

후처리

  1. temperatureunder heat-refluxing for 6 hours
  2. concentrationThe reaction liquor was concentrated
  3. addition100 ml of water was added
  4. temperatureunder cooling with ice
  5. extractionwas extracted twice with 100 ml of diethyl ether
  6. washThe extracted liquor was washed with water
  7. dry with materialwas dried with anhydrous sodium sulfate for one night
  8. filtrationAfter filtrating the inorganic salt
  9. distillationthe solvent was distilled off under reduced pressure
  10. customto obtain 5.8 g of a crude crystal
  11. customThe crude crystal thus obtained
  12. customwas recrystallized from ether-hexane

출처 및 근거

ORD 기록
ord-15f740dd779b4fa4b741e4a596bcf2d4
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05411934

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