硫酸氢钠 → 2-(2-trifluoromethyl-phenyl)-3H-pyrido[2,3-d]pyrimidin-4-one

HRID 38173

反应方程式

HRID 38173 反应方程式
[F:1][C:2]([F:22])([F:21])[C:3]1[CH:20]=[CH:19][CH:18]=[CH:17][C:4]=1[C:5]([NH:7][C:8]1[N:16]=[CH:15][CH:14]=[CH:13][C:9]=1[C:10]([NH2:12])=[O:11])=O.[O-]CC.[K+].S([O-])(O)(=O)=O.[Na+]>C(O)C.O>[F:1][C:2]([F:22])([F:21])[C:3]1[CH:20]=[CH:19][CH:18]=[CH:17][C:4]=1[C:5]1[NH:12][C:10](=[O:11])[C:9]2[CH:13]=[CH:14][CH:15]=[N:16][C:8]=2[N:7]=1

参与物

6

反应物 3

HCID 516919硫酸氢钠HCID 219392142-[2-(Trifluoromethyl)benzamido]pyridine-3-carboxamideHCID 23670592乙醇钾

产物 1

HCID 1358508342-(2-trifluoromethyl-phenyl)-3H-pyrido[2,3-d]pyrimidin-4-one

试剂、催化剂与溶剂 2

HCID 702乙醇溶剂HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

实验过程

2-(2-Trifluoromethyl-benzoylamino)-nicotinamide (800 mg, 2.6 mmol) is dissolved in 10 ml of ethanol. Potassium ethoxide (435 mg, 5.2 mmol) is added to the solution which is heated to reflux for 16 h. The reaction mixture is evaporated in vacuo to afford a gummy residue that is dissolved in water and acidified with 10% sodium hydrogen sulfate to pH 7. The resulting precipitate is filtered and dried under vacuum at 50 C to give 2-(2-trifluoromethyl-phenyl)-3H-pyrido[2,3-d]pyrimidin-4-one.

后处理

  1. temperatureis heated
  2. temperatureto reflux for 16 h
  3. customThe reaction mixture is evaporated in vacuo
  4. customto afford a gummy residue that
  5. filtrationThe resulting precipitate is filtered
  6. customdried under vacuum at 50 C

来源与证据

ORD记录
ord-021814edc3f74ffab715b58d6995521d
来源数据集
uspto-grants-2013_09
专利号
US08524720B2

关联笔记

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