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Acetic Acid → 2-(methylsulfinyl)-3-[4-(2,2,2-trifluoroethoxy)phenyl]pyrido[2,3-d]pyrimidine-4,7(3H,8H)-dione

HRID 570693
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HRID 570693 반응식
[CH3:1][S:2][C:3]1[N:4]([C:15]2[CH:20]=[CH:19][C:18]([O:21][CH2:22][C:23]([F:26])([F:25])[F:24])=[CH:17][CH:16]=2)[C:5](=[O:14])[C:6]2[CH:12]=[CH:11][C:10](=[O:13])[NH:9][C:7]=2[N:8]=1.C(O)(=[O:29])C>O>[CH3:1][S:2]([C:3]1[N:4]([C:15]2[CH:16]=[CH:17][C:18]([O:21][CH2:22][C:23]([F:24])([F:26])[F:25])=[CH:19][CH:20]=2)[C:5](=[O:14])[C:6]2[CH:12]=[CH:11][C:10](=[O:13])[NH:9][C:7]=2[N:8]=1)=[O:29]
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참가 물질

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반응물 2

HCID 176Acetic AcidHCID 866853542-(methylsulfanyl)-3-[4-(2,2,2-trifluoroethoxy)phenyl]pyrido[2,3-d]pyrimidine-4,7(3H,8H)-dione

생성물 1

HCID 866853562-(methylsulfinyl)-3-[4-(2,2,2-trifluoroethoxy)phenyl]pyrido[2,3-d]pyrimidine-4,7(3H,8H)-dione

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

2-(Methylsulfanyl)-3-[4-(2,2,2-trifluoroethoxy)phenyl]pyrido[2,3-d]pyrimidine-4,7(3H,8H)-dione (505 mg) was dissolved in acetic acid (12 ml), and a solution of oxoso (registered mark) (1.05 g) in water (3 ml) was added thereto, and the mixture was stirred at room temperature for 1 hr. To the reaction mixture was added water (50 ml), and the white precipitate was collected by filtration, and washed with diisopropyl ether. The obtained solid was dried under reduced pressure, and subjected to azeotropic distillation with acetonitrile to give the title compound (528 mg) as a white solid.

후처리

  1. filtrationthe white precipitate was collected by filtration
  2. washwashed with diisopropyl ether
  3. customThe obtained solid was dried under reduced pressure
  4. distillationsubjected to azeotropic distillation with acetonitrile

출처 및 근거

ORD 기록
ord-d935df36f36047f99ca9932dbbb38ecd
출처 데이터셋
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09023858B2

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