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

HRID 25867ノート

反応式

HRID 25867 の反応式
[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]

参加物

6

反応物 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

生成物 1

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

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 80711,2-Dimethoxyethane溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-3daef18a793e446e9d422b3c51603dd1
出典データセット
uspto-grants-1979_04
特許番号
US04147528

反応ノート

読み込み中…