3-Ethoxy-3-oxo-2-phenylpropanoic acid → HCID 178517418、化合物

HRID 2267992

反応式

HRID 2267992 の反応式
[Na].Cl.[Br:3][C:4]1[CH:12]=[CH:11][C:7]([C:8]([NH2:10])=[NH:9])=[CH:6][CH:5]=1.C([O:15][C:16](=O)[CH:17]([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[C:18](O)=[O:19])C>CO>[Br:3][C:4]1[CH:12]=[CH:11][C:7]([C:8]2[N:10]=[C:18]([OH:19])[C:17]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)=[C:16]([OH:15])[N:9]=2)=[CH:6][CH:5]=1

参加物

5

反応物 3

HCID 27299033-Ethoxy-3-oxo-2-phenylpropanoic acidHCID 5360545SodiumHCID 122077144-Bromobenzene-1-carboximidamide--hydrogen chloride (1/1)

生成物 1

HCID 178517418HCID 178517418、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
80 °C

実験手順

Into a solution of 3.45 g (150 mmol) of sodium in 100 ml methanol, here were sequentially added 10.98 g (47 mmol) 4-bromobenzamidine hydrochloride and 11.15 g (47 mmol) of phenyl malonic acid ethyl ester. The mixture was heated for 12 hours at 80° C. The deep yellow reaction solution was filtered to remove the precipitated sodium chloride and thereafter the pyrimidine was precipitated with 10 ml of 2 molar hydrochloric acid as an intensive yellow solid. The solid was sequentially washed with water, ethanol and diethyl ether. Yield: 12.70 g (37 mmol, 79% theory) of yellow solid. The pyrimidine is insoluble in all tested organic solvents as well as in water. m.p. greater >230° C.

後処理

  1. filtrationThe deep yellow reaction solution was filtered
  2. customto remove the precipitated sodium chloride
  3. customthe pyrimidine was precipitated with 10 ml of 2 molar hydrochloric acid as an intensive yellow solid
  4. washThe solid was sequentially washed with water, ethanol and diethyl ether
  5. customm.p. greater >230° C.

出典と根拠

ORDレコード
ord-450dc10b50984b4aa5ddbde196c4908c
出典データセット
uspto-grants-2001_12
特許番号
US06326327B1

関連ノート

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