Methanol → 4,6-Dimethoxy-2-(p-tolyl)pyrimidine

HRID 652994ノート

反応式

HRID 652994 の反応式
[CH3:1][O-:2].[Na+].[C:4]1([CH3:18])[CH:9]=[CH:8][C:7]([C:10]2[N:15]=[C:14](Cl)[CH:13]=[C:12](Cl)[N:11]=2)=[CH:6][CH:5]=1.[CH3:19][OH:20]>>[C:4]1([CH3:18])[CH:9]=[CH:8][C:7]([C:10]2[N:15]=[C:14]([O:2][CH3:1])[CH:13]=[C:12]([O:20][CH3:19])[N:11]=2)=[CH:6][CH:5]=1

参加物

4

反応物 3

HCID 887MethanolHCID 10942334Sodium MethoxideHCID 12703697HCID 12703697、化合物

生成物 1

HCID 127036994,6-Dimethoxy-2-(p-tolyl)pyrimidine

実験手順

156.1 g of a 30.5% solution of sodium methylate are stirred with 700 ml of anhydrous methanol. To the solution are then added, over 10 minutes and with gentle cooling, 95.64 g of 2-p-tolyl-4,6-dichloropyrimidine. The mixture is then heated to reflux and kept at the boil for 4 hours. The solvent is removed by distillation and the residue is charged into 1000 ml of water. The product is triturated with water to remove sodium chloride, isolated by filtration, washed with water and dried in the air, affording 90.4 g of the title compound with a melting point of 61°-62° C.

後処理

  1. temperatureThe mixture is then heated
  2. temperatureto reflux
  3. customThe solvent is removed by distillation
  4. additionthe residue is charged into 1000 ml of water
  5. customThe product is triturated with water
  6. customto remove sodium chloride
  7. customisolated by filtration
  8. washwashed with water
  9. customdried in the air

出典と根拠

ORDレコード
ord-8abae1d2b19d4dbba2c8f3189a1a1581
出典データセット
uspto-grants-1987_06
特許番号
US04674229

反応ノート

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