Water → HCID 15059441、化合物

HRID 36844ノート

反応式

HRID 36844 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 15059441HCID 15059441、化合物収率 75.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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 bottomed 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.

後処理

  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

出典と根拠

ORDレコード
ord-906e0f3aee264c5d9a0fd6653d203ce0
出典データセット
uspto-grants-1995_05
特許番号
US05418212

反応ノート

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