Phosphorus oxychloride → 3-benzyl-6-chloro-5-methylpyrimidine-2,4(1H,3H)-dione

HRID 357108

반응식

HRID 357108 반응식
P(Cl)(Cl)([Cl:3])=O.[CH2:6]([N:13]1[C:18](=[O:19])[CH:17]([CH3:20])[C:16](=O)[NH:15][C:14]1=[O:22])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1>C(O)C>[CH2:6]([N:13]1[C:18](=[O:19])[C:17]([CH3:20])=[C:16]([Cl:3])[NH:15][C:14]1=[O:22])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

참가 물질

4

반응물 2

HCID 24813Phosphorus oxychlorideHCID 189367221-Benzyl-5-methyl-pyrimidine-2,4,6-trione

생성물 1

HCID 189368853-benzyl-6-chloro-5-methylpyrimidine-2,4(1H,3H)-dione

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To 16.8 ml of 50% ethanol, 78.7 ml (844 mmol) of phosphorus oxychloride was added dropwise, with stirring under ice cooling conditions. To this solution, 23.22 g (100 mmol) of 3-benzyl-5-methylpyrimidine-2,4,6(1H,3H)-trione was added little by little. This mixture was stirred at 50° C. for 30 minutes and then at 100° C. for 90 minutes. After cooling, the reaction mixture was poured into ice water and stirred for 1 hour. The resulting precipitate was collected by filtration, washed with water and n-hexane and dried to yield 27.50 g (quant, light white crystal) of the desired product.

후처리

  1. stirringThis mixture was stirred at 50° C. for 30 minutes
  2. temperatureAfter cooling
  3. stirringstirred for 1 hour
  4. filtrationThe resulting precipitate was collected by filtration
  5. washwashed with water and n-hexane
  6. customdried

출처 및 근거

ORD 기록
ord-fed3e0ea75bf47e29a61d6f7b0c21785
출처 데이터셋
uspto-grants-1998_11
특허 번호
US05840732

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