三氯氧磷 → Methyl 4-((2-amino-4-chloro-6-methylpyrimidin-5-yl)methyl)-3-methoxybenzoate

HRID 1617153笔记

反应方程式

HRID 1617153 反应方程式
[NH2:1][C:2]1[N:7]=[C:6](O)[C:5]([CH2:9][C:10]2[CH:19]=[CH:18][C:13]([C:14]([O:16][CH3:17])=[O:15])=[CH:12][C:11]=2[O:20][CH3:21])=[C:4]([CH3:22])[N:3]=1.P(Cl)(Cl)([Cl:25])=O>>[NH2:1][C:2]1[N:7]=[C:6]([Cl:25])[C:5]([CH2:9][C:10]2[CH:19]=[CH:18][C:13]([C:14]([O:16][CH3:17])=[O:15])=[CH:12][C:11]=2[O:20][CH3:21])=[C:4]([CH3:22])[N:3]=1

参与物

3

反应物 2

HCID 24813三氯氧磷HCID 178497678HCID 178497678，化合物

产物 1

HCID 86633398Methyl 4-((2-amino-4-chloro-6-methylpyrimidin-5-yl)methyl)-3-methoxybenzoate

反应条件

温度
100 °C

实验过程

The product from step (ii) (8.6 g) was added to phosphorous oxychloride (50 ml) and the resulting suspension stirred at 100° C. for 15 h. The reaction mixture was allowed to cool and the phosphorous oxychloride evaporated under reduced pressure. The residue was diluted with water (100 mL) and the suspension adjusted to pH 7 with NaHCO3. The mixture was heated at 50° C. for 1 h and allowed to cool. The solid was collected by filtration, washed with water, EtOAc and dried under vacuum to give the subtitle compound 9.05 g.

后处理

  1. temperatureto cool
  2. customthe phosphorous oxychloride evaporated under reduced pressure
  3. additionThe residue was diluted with water (100 mL)
  4. temperatureThe mixture was heated at 50° C. for 1 h
  5. temperatureto cool
  6. filtrationThe solid was collected by filtration
  7. washwashed with water, EtOAc
  8. customdried under vacuum

来源与证据

ORD记录
ord-903aad2253ce4ddc934d4863b19c0daa
来源数据集
uspto-grants-2014_07
专利号
US08765939B2

反应笔记

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