Diethyl Malonate → HCID 178483102、化合物

HRID 2419640ノート

反応式

HRID 2419640 の反応式
S(O)(O)(=O)=O.[CH3:6][N:7]([CH3:11])[C:8]([NH2:10])=[NH:9].C[O-].[Na+].C([O:17][C:18](=O)[CH2:19][C:20](OCC)=[O:21])C>CO>[CH3:6][N:7]([CH3:11])[C:8]1[N:10]=[C:18]([OH:17])[CH:19]=[C:20]([OH:21])[N:9]=1

参加物

5

反応物 3

HCID 7761Diethyl MalonateHCID 220673Guanidine, 1,1-dimethyl-, sulfateHCID 10942334Sodium Methoxide

生成物 1

HCID 178483102HCID 178483102、化合物収率 96.7%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

136 g (0.5 mol) of N,N-dimethylguanidine sulphate were added to a solution of 162 g (3 mol) of sodium methylate in 1 l of methanol at 0° to 5° C. 160 g (1 mol) of malonic acid diethyl ester were then allowed to run in without cooling and the mixture was stirred for 24 hours at room temperature. The solvent was then distilled off in vacuo and the residue was dissolved in water. The solution was brought to approximately pH 5 by adding glacial acetic acid; it was then cooled to 0°-5° C and the product which had precipitated was filtered off. 75 g (48% of theory) of 2-dimethylamino-4,6-dihydroxypyrimidine were thus obtained in the form of a colorless powder of melting point > 300° C.

後処理

  1. temperaturewithout cooling
  2. distillationThe solvent was then distilled off in vacuo
  3. dissolutionthe residue was dissolved in water
  4. additionby adding glacial acetic acid
  5. temperatureit was then cooled to 0°-5° C
  6. customthe product which had precipitated
  7. filtrationwas filtered off

出典と根拠

ORDレコード
ord-5fa7fbcd51f542c6b883cd0cfef7ea3e
出典データセット
uspto-grants-1978_08
特許番号
US04107301

反応ノート

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