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

HRID 357115

반응식

HRID 357115 반응식
P(Cl)(Cl)([Cl:3])=O.[CH2:6]([N:13]1[C:18](=[O:19])[CH:17]([CH2:20][C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[C:16](=O)[NH:15][C:14]1=[O:28])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1>C(O)C>[Cl:3][C:16]1[NH:15][C:14](=[O:28])[N:13]([CH2:6][C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[C:18](=[O:19])[C:17]=1[CH2:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1

참가 물질

4

반응물 2

HCID 24813Phosphorus oxychlorideHCID 2687313,5-dibenzylpyrimidine-2,4,6(1H,3H)-trione

생성물 1

HCID 189366616-chloro-3,5-dibenzylpyrimidine-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 drop by drop, with stirring under ice cooling conditions. To this solution, 30.83 g (100 mmol) of 3,5-dibenzylpyrimidine-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 32.62 g (99.8%, 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-95574b1b83ac4a4db004997c82ad10ad
출처 데이터셋
uspto-grants-1998_11
특허 번호
US05840732

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