Sodium hydride → Sodium 1,6-dihydro-4-methyl-6-oxo-1-(4-tolyl)pyrimidine-5-carboxylate

HRID 25867노트

반응식

HRID 25867 반응식
[CH3:1][C:2]1[N:3]=[CH:4][N:5]([C:12]2[CH:17]=[CH:16][C:15]([CH3:18])=[CH:14][CH:13]=2)[C:6](=[O:11])[C:7]=1[C:8]([OH:10])=[O:9].CC1N=CN(C2C=CC(C)=CC=2)C(=O)C=1C(OCC)=O.[H-].[Na+:40]>C(COC)OC.CCOCC>[CH3:1][C:2]1[N:3]=[CH:4][N:5]([C:12]2[CH:13]=[CH:14][C:15]([CH3:18])=[CH:16][CH:17]=2)[C:6](=[O:11])[C:7]=1[C:8]([O-:10])=[O:9].[Na+:40]

참가 물질

6

반응물 3

HCID 24758Sodium hydrideHCID 213254901,6-Dihydro-4-methyl-6-oxo-1-(4-tolyl)pyrimidine-5-carboxylic acidHCID 21325495Ethyl 1,6-dihydro-4-methyl-6-oxo-1-(4-tolyl)pyrimidine-5-carboxylate

생성물 1

HCID 23684865Sodium 1,6-dihydro-4-methyl-6-oxo-1-(4-tolyl)pyrimidine-5-carboxylate수율 57%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 80711,2-Dimethoxyethane용매

실험 절차

A mixture of 8.0 g (0.033 mole) of 1,6-dihydro-4-methyl-6-oxo-1-(4-tolyl)pyrimidine-5-carboxylic acid, prepared from ethyl 1,6-dihydro-4-methyl-6-oxo-1-(4-tolyl)pyrimidine-5-carboxylate by the hydrolysis method of Example 2, and one equivalent of sodium hydride (added as mineral oil dispersion), slurried in 300 ml of glyme is stirred at ambient temperature for 3 days. The solid product is isolated by filtration, slurried in ether and reisolated to give after drying 5.0 g (57% yield) of sodium 1,6-dihydro-4-methyl-6-oxo-1-(4-tolyl)pyrimidine-5-carboxylate, m.p. 208°-10° C. dec.

후처리

  1. customThe solid product is isolated by filtration
  2. customto give

출처 및 근거

ORD 기록
ord-3daef18a793e446e9d422b3c51603dd1
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04147528

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