Sodium Hydroxide → 4-Chloro-6-methyl-2-(propan-2-yl)pyrimidine

HRID 14345

반응식

HRID 14345 반응식
[CH:1]([C:4]1[N:9]=[C:8](O)[CH:7]=[C:6]([CH3:11])[N:5]=1)([CH3:3])[CH3:2].P(Cl)(Cl)([Cl:14])=O.[OH-].[Na+]>C1(C)C=CC=CC=1>[Cl:14][C:8]1[CH:7]=[C:6]([CH3:11])[N:5]=[C:4]([CH:1]([CH3:3])[CH3:2])[N:9]=1

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 24813Phosphorus oxychlorideHCID 178419104HCID 178419104, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
110 °C

실험 절차

76.1 g of 2-isopropyl-6-methyl-4-pyrimidinol [2814-20-2] (500 mmol) are dissolved in 300 ml of toluene at 90° C. 80.5 g of phosphorus oxychloride (525 mmol) are added dropwise thereto at from 90 to 103° C., and the reaction mixture is heated at 110° C. for 2 hours. After cooling to 20° C., the reaction mixture is adjusted to pH 8 using 4M sodium hydroxide solution, with cooling. The aqueous phase is separated off and extracted with 100 ml of toluene. The combined organic phases are washed three times with 100 ml of water each time and dried at RT under 2 mbar. 89.7 g (105%; contains toluene) are obtained.

후처리

  1. temperatureAfter cooling to 20° C.
  2. temperaturewith cooling
  3. customThe aqueous phase is separated off
  4. extractionextracted with 100 ml of toluene
  5. washThe combined organic phases are washed three times with 100 ml of water each time
  6. customdried at RT under 2 mbar
  7. custom89.7 g (105%; contains toluene) are obtained

출처 및 근거

ORD 기록
ord-c1733baf1fbe4d7cba07485c4f3375fa
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07731985B2

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