Dimethyl Sulfoxide → N-(Hexahydro-1,5-dimethyl-2,4,6-trioxo-5-pyrimidinyl)-2,3,4,5-tetrafluorobenzamide

HRID 1097278노트

반응식

HRID 1097278 반응식
Cl.[NH2:2][C:3]1([CH3:13])[C:8](=[O:9])[N:7]([CH3:10])[C:6](=[O:11])[NH:5][C:4]1=[O:12].[F:14][C:15]1[C:16]([F:28])=[C:17]([F:27])[C:18]([F:26])=[C:19]2C(=O)O[C:21](=[O:22])[C:20]=12.CCN(CC)CC.CS(C)=O>O>[CH3:10][N:7]1[C:8](=[O:9])[C:3]([NH:2][C:21](=[O:22])[C:20]2[CH:19]=[C:18]([F:26])[C:17]([F:27])=[C:16]([F:28])[C:15]=2[F:14])([CH3:13])[C:4](=[O:12])[NH:5][C:6]1=[O:11]

참가 물질

6

반응물 4

HCID 679Dimethyl SulfoxideHCID 8471TriethylamineHCID 69545Tetrafluorophthalic anhydrideHCID 66811031HCID 66811031, 화합물

생성물 1

HCID 24765565N-(Hexahydro-1,5-dimethyl-2,4,6-trioxo-5-pyrimidinyl)-2,3,4,5-tetrafluorobenzamide

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
153 °C

실험 절차

A mixture of 5-amino-1,5-dimethylbarbituric acid hydrochloride (0.42 g, 2 mmol), tetrafluorophthalic anhydride (0.44 g, 2 mmol), Et3N (0.28 mL, 0.20 g, 2 mmol) and DMSO (3 mL) was stirred and heated at 153° C. for 5 hours. The reaction mixture was then allowed to cool down to room temperature and poured into water (10 mL). The oil that immediately formed was carefully removed from the solution, from which a solid precipitated after 4 days standing at room temperature. The precipitate was collected by filtration, washed with water and dried under reduced pressure to give 20a as yellow crystals.

후처리

  1. temperatureto cool down to room temperature
  2. customThe oil that immediately formed
  3. customwas carefully removed from the solution, from which a solid
  4. customprecipitated after 4 days
  5. customstanding at room temperature
  6. filtrationThe precipitate was collected by filtration
  7. washwashed with water
  8. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-63e15b5ce3de44278155a60744c3de3c
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08143252B2

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