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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
ノート
印刷プレビュー

反応式

HRID 570693 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d935df36f36047f99ca9932dbbb38ecd
出典データセット
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09023858B2

反応ノート

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