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Dimethyl Sulfoxide → 6-(2,6-Dichlorophenyl)-8-methyl-2-methylsulfonyl-8H-pyrido[2,3-d]pyrimidin-7-one

HRID 3181
ノート
印刷プレビュー

反応式

HRID 3181 の反応式
ClC1C=CC=C(C(OO)=[O:9])C=1.[Cl:12][C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([Cl:19])[C:14]=1[C:20]1[C:31](=[O:32])[N:30]([CH3:33])[C:23]2[N:24]=C(SC)[N:26]=[CH:27][C:22]=2[CH:21]=1.[CH3:34][S:35]([CH3:37])=[O:36]>C(Cl)(Cl)Cl>[Cl:12][C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([Cl:19])[C:14]=1[C:20]1[C:31](=[O:32])[N:30]([CH3:33])[C:23]2[N:24]=[C:34]([S:35]([CH3:37])(=[O:9])=[O:36])[N:26]=[CH:27][C:22]=2[CH:21]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 679Dimethyl SulfoxideHCID 70297m-Chloroperbenzoic acidHCID 107367016-(2,6-Dichlorophenyl)-8-methyl-2-(methylthio)pyrido[2,3-d]pyrimidin-7(8H)-one

生成物 1

HCID 105961576-(2,6-Dichlorophenyl)-8-methyl-2-methylsulfonyl-8H-pyrido[2,3-d]pyrimidin-7-one

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

A quantity of 0.346 g (1.00 mmol) of 50% to 60% m-chloroperbenzoic acid (assuming 50% peracid was present) was added at 25° C. to a stirred solution of 0.165 g (0.47 mmol) of 6-(2,6-dichlorophenyl)-8-methyl-2-methylsulfanyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 37 in 15 mL of chloroform, and the solution was stirred overnight. A quantity of 0.25 g (3.20 mmol) of dimethylsulfoxide was added to reduce any excess peracid. After 15 minutes, the chloroform solution was washed with 30 mL of saturated sodium bicarbonate and then with water. The separated organic layer was dried over sodium sulfate, filtered, and concentrated to ca. 5 mL volume. Crystals separated. Added ca. 5 mL of petroleum ether and filtered; wt 0.165 g (92%); mp >290° C.

後処理

  1. waitAfter 15 minutes
  2. washthe chloroform solution was washed with 30 mL of saturated sodium bicarbonate
  3. dry with materialThe separated organic layer was dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated to ca. 5 mL volume
  6. customCrystals separated
  7. additionAdded ca. 5 mL of petroleum ether
  8. filtrationfiltered

出典と根拠

ORDレコード
ord-bfb87e53646f4c08bf6331ebf2a578a0
出典データセット
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05733914

反応ノート

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