Dichloromethane → 4,6-Dichloro-2-methylpyrimidine

HRID 19504

反応式

HRID 19504 の反応式
O[C:2]1[CH:7]=C(O)[N:5]=[C:4]([CH3:9])[N:3]=1.P(Cl)(Cl)([Cl:12])=O.Cl[CH2:16][Cl:17]>>[Cl:12][C:2]1[CH:7]=[C:16]([Cl:17])[N:5]=[C:4]([CH3:9])[N:3]=1

参加物

4

反応物 3

HCID 6344DichloromethaneHCID 24813Phosphorus oxychlorideHCID 178418389HCID 178418389、化合物

生成物 1

HCID 2349974,6-Dichloro-2-methylpyrimidine

反応条件

温度
95 °C

実験手順

4,6-Dihydroxy-2-methylpyrimidine 21 (1.03 g, 8.1 mmol) is suspended in 2.5 mL phosphorus oxychloride (27.3 mmol). The mixture is heated to 95° C. for 18 hours. Upon cooling, the mixture is diluted with dichloromethane (100 mL) and filtered. It is then washed with water, saturated aqueous sodium bicarbonate and brine, then concentrated to yield 4,6-dichloro-2-methylpyrimidine 22 as a white powder. 1H-NMR (400 MHz, CDCl3) δ=7.45 (s, 1H), 2.77 (s, 3H). MS calculated for C5H5Cl2N2 (M+H+) 162.99. found 163.2.

後処理

  1. temperatureUpon cooling
  2. filtrationfiltered
  3. washIt is then washed with water, saturated aqueous sodium bicarbonate and brine
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-9f9d73ccab04499d925e69c5dfa51904
出典データセット
uspto-grants-2010_06
特許番号
US07745445B2

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