Phosphorus oxychloride → Ethyl 4-chloro-2-ethylpyrimidine-5-carboxylate

HRID 1413436ノート

反応式

HRID 1413436 の反応式
P(Cl)(Cl)([Cl:3])=O.[CH2:6]([O:8][C:9]([C:11]1[C:12](O)=[N:13][C:14]([CH2:17][CH3:18])=[N:15][CH:16]=1)=[O:10])[CH3:7]>C(N(CC)CC)C>[CH2:6]([O:8][C:9]([C:11]1[C:12]([Cl:3])=[N:13][C:14]([CH2:17][CH3:18])=[N:15][CH:16]=1)=[O:10])[CH3:7]

参加物

4

反応物 2

HCID 24813Phosphorus oxychlorideHCID 178469771HCID 178469771、化合物

生成物 1

HCID 12363083Ethyl 4-chloro-2-ethylpyrimidine-5-carboxylate

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

反応条件

温度
0 °C

実験手順

7.5 ml of triethylamine were slowly introduced into 300 ml of phosphorous oxychloride cooled to 0° C., then were added 30 g of 5-ethoxycarbonyl 4-hydroxy 2-ethyl pyrimidine (VII) prepared in the preceding stage and the suspension was brought up to 40° C. under nitrogen scavenging. After dissolution, the phosphorous oxychloride was evaporated and the residue diluted in a mixture of water and chloroform. This was decanted, the chloroform phase was twice washed with water, dried on sodium sulfate and the solvent evaporated. The raw product obtained, after checking the purity by thin layer chromatography, was reacted in the following stage 3.

後処理

  1. customprepared in the preceding stage
  2. customwas brought up to 40° C. under nitrogen scavenging
  3. dissolutionAfter dissolution
  4. customthe phosphorous oxychloride was evaporated
  5. additionthe residue diluted in a mixture of water and chloroform
  6. customThis was decanted
  7. washthe chloroform phase was twice washed with water
  8. customdried on sodium sulfate
  9. customthe solvent evaporated

出典と根拠

ORDレコード
ord-ffd9be3dd206450d9b6d8d96b70394b1
出典データセット
uspto-grants-1981_02
特許番号
US04250178

反応ノート

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