6-(2,6-Dichlorophenyl)-8-methyl-2-methylsulfonyl-8H-pyrido[2,3-d]pyrimidin-7-one → HCID 17747295、化合物

HRID 1176194

反応式

HRID 1176194 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[C:9]1[C:22](=[O:23])[N:21]([CH3:24])[C:12]2[N:13]=[C:14](S(C)(=O)=O)[N:15]=[CH:16][C:11]=2[CH:10]=1.[CH2:25]1[C:33]2[C:28](=[CH:29][C:30]([NH2:34])=[CH:31][CH:32]=2)[CH2:27][O:26]1>C(O)(=O)C>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[C:9]1[C:22](=[O:23])[N:21]([CH3:24])[C:12]2[N:13]=[C:14]([NH:34][C:30]3[CH:29]=[C:28]4[C:33](=[CH:32][CH:31]=3)[CH2:25][O:26][CH2:27]4)[N:15]=[CH:16][C:11]=2[CH:10]=1

参加物

4

反応物 2

HCID 105961576-(2,6-Dichlorophenyl)-8-methyl-2-methylsulfonyl-8H-pyrido[2,3-d]pyrimidin-7-oneHCID 124453391,3-Dihydro-2-benzofuran-5-amine

生成物 1

HCID 17747295HCID 17747295、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A mixture of 0.614 g of compound of formula (II), 6-(2,6-dichlorophenyl)-8-methyl-2-methylsulfonyl-8H-pyrido[2,3-d]pyrimidin-7-one, and 0.389 g of the compound of formula (III), (1,3-dihydro-5-isobenzofuranyl)amine, is heated in 10 ml of acetic acid at reflux for 20 min; the reaction medium is concentrated by half under vacuum, then taken up in a mixture of ethyl acetate and water and brought to pH 9 with a saturated NaHCO3 solution. After separating by settling, the organic phase is washed with water and then with a saturated NaCl solution, dried over sodium sulfate and then evaporated to dryness. The product is purified by flash chromatography on silica with a gradient of 0 to 50% of ethyl acetate in dichloromethane. 0.140 g of expected product is obtained in the form of a yellow solid.

後処理

  1. temperatureat reflux for 20 min
  2. concentrationthe reaction medium is concentrated by half under vacuum
  3. additiontaken up in a mixture of ethyl acetate and water
  4. customAfter separating
  5. washthe organic phase is washed with water
  6. dry with materialwith a saturated NaCl solution, dried over sodium sulfate
  7. customevaporated to dryness
  8. customThe product is purified by flash chromatography on silica with a gradient of 0 to 50% of ethyl acetate in dichloromethane

出典と根拠

ORDレコード
ord-ee06d7e728cd4696bf710bdb21d6b1ce
出典データセット
uspto-grants-2010_11
特許番号
US07842806B2

関連ノート

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