Phosphorus oxychloride → 4-Chloro-6-methyl-2-(propan-2-yl)pyrimidine

HRID 1380842

反応式

HRID 1380842 の反応式
O[C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]([CH:9]([CH3:11])[CH3:10])[N:3]=1.P(Cl)(Cl)([Cl:14])=O>C(Cl)(Cl)Cl>[Cl:14][C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]([CH:9]([CH3:11])[CH3:10])[N:3]=1

参加物

4

反応物 2

HCID 24813Phosphorus oxychlorideHCID 178419104HCID 178419104、化合物

生成物 1

HCID 33069074-Chloro-6-methyl-2-(propan-2-yl)pyrimidine

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

A mixture of 6.5 g (0.036 mol) of 4-hydroxy-2-isopropyl-6-methyl-pyrimidine and 16.8 g (0.108 mol) of phosphorus oxychloride in 40 ml of chloroform is heated at reflux for 2 hours. The solution is then concentrated under reduced pressure, the residue is poured into water and the aqueous phase is extracted twice with 100 ml of n-hexane each time. The organic phase is dried over anhydrous sodium sulphate and subsequently evaporated. There is obtained 4-chloro-2-isopropyl-6-methyl-pyrimidine in the form of an orange oil, 1H-NMR (CDCl3): 1.32 (d, CH(CH3)2), 2.48 (s, CH3), 3.17 (m, CH(CH3)2), 7.03 (s, CH).

後処理

  1. temperatureis heated
  2. temperatureat reflux for 2 hours
  3. concentrationThe solution is then concentrated under reduced pressure
  4. additionthe residue is poured into water
  5. extractionthe aqueous phase is extracted twice with 100 ml of n-hexane each time
  6. dry with materialThe organic phase is dried over anhydrous sodium sulphate
  7. customsubsequently evaporated

出典と根拠

ORDレコード
ord-fdc704a5a1e9446c90a1510fcc209d70
出典データセット
uspto-grants-1986_04
特許番号
US04584295

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