Sodium Hydroxide → 2-Methoxy-6-methylpyrimidine-4-carboxylic acid

HRID 1109978노트

반응식

HRID 1109978 반응식
[CH3:1][O:2][C:3]1[N:8]=[C:7]([C:9]([O:11]C)=[O:10])[CH:6]=[C:5]([CH3:13])[N:4]=1.[OH-].[Na+]>CO.O>[CH3:1][O:2][C:3]1[N:8]=[C:7]([C:9]([OH:11])=[O:10])[CH:6]=[C:5]([CH3:13])[N:4]=1

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 19018471Methyl 2-methoxy-6-methylpyrimidine-4-carboxylate

생성물 1

HCID 190184722-Methoxy-6-methylpyrimidine-4-carboxylic acid수율 46.1%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

15.5 g of methyl 2-methoxy-6-methylpyrimidine-4-carboxylate are added to a stirred solution of 3.6 g of sodium hydroxide in 100 ml of methanol and 10 ml of water. Stirring is continued at room temperature until the starting material disappears (TLC checking; 3 h). The methanol is distilled off under reduced pressure, the residue is taken up in water and the mixture is extracted once with ethyl acetate. The aqueous phase is acidified to pH 2 with conc. hydrochloric acid and then stirred for 1 h, and the product is filtered off with suction. 6.6 g of 2-methoxy-6-methylpyrimidine-4-carboxylic acid of melting point 161°-163° C. are obtained in this way. Concentration and extraction of the mother liquor using dichloromethane additionally gives 3.1 g of product of melting point 159°-161° C.

후처리

  1. customis continued at room temperature until the starting material
  2. custom(TLC checking; 3 h)
  3. distillationThe methanol is distilled off under reduced pressure
  4. extractionthe mixture is extracted once with ethyl acetate
  5. stirringstirred for 1 h
  6. filtrationthe product is filtered off with suction

출처 및 근거

ORD 기록
ord-4bb449d3169a43248c0fc265a6e2b90d
출처 데이터셋
uspto-grants-1994_06
특허 번호
US05324710

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