Methyl 4-chloroacetoacetate → HCID 178467470、化合物

HRID 1380846ノート

反応式

HRID 1380846 の反応式
Cl.[CH2:2]([O:4][C:5](=[NH:7])[NH2:6])[CH3:3].[Cl:8][CH2:9][C:10](=O)[CH2:11][C:12](OC)=[O:13].[Na]>CO>[CH2:2]([O:4][C:5]1[N:6]=[C:10]([CH2:9][Cl:8])[CH:11]=[C:12]([OH:13])[N:7]=1)[CH3:3]

参加物

5

反応物 3

HCID 36240Methyl 4-chloroacetoacetateHCID 5360545SodiumHCID 122987352-Ethylisouronium chloride

生成物 1

HCID 178467470HCID 178467470、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

反応条件

温度
0 °C

実験手順

A mixture of 24.9 g (0.2 mol) of O-ethylisourea hydrochloride and 21.5 g (0.14 mol) of methyl 4-chloroacetoacetate in 100 ml of methanol is treated at 0°-5° C. during 10 minutes with a solution of 7.55 g (0.33 mol) of sodium in 100 ml of methanol. The mixture is stirred at 0° C. for 2 hours and at room temperature for 18 hours and the solvent is then removed by evaporation under reduced pressure. The residue is dissolved in 300 ml of water and the solution is adjusted to a pH-value of 6. The resulting crystallline product is filtered off, washed with diethyl ether and dried at 40° C. In this manner there is obtained 2-ethoxy-4-chloromethyl-6-hydroxy-pyrimidine, m.p. 157°-159° C. By back-extracting the aqueous filtrate three times with 150 ml of chloroform each time there is obtained an additional amount of this product, m.p. 159°-161° C.

後処理

  1. customthe solvent is then removed by evaporation under reduced pressure
  2. dissolutionThe residue is dissolved in 300 ml of water
  3. filtrationThe resulting crystallline product is filtered off
  4. washwashed with diethyl ether
  5. customdried at 40° C

出典と根拠

ORDレコード
ord-c922cc9b35e54dfa8bc53a909857f975
出典データセット
uspto-grants-1986_04
特許番号
US04584295

反応ノート

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