Phosphorus oxychloride → Methyl 4-((2-amino-4-chloro-6-methylpyrimidin-5-yl)methyl)-3-methoxybenzoate

HRID 1617153

反応式

HRID 1617153 の反応式
[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

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 178497678HCID 178497678、化合物

生成物 1

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

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-903aad2253ce4ddc934d4863b19c0daa
出典データセット
uspto-grants-2014_07
特許番号
US08765939B2

関連ノート

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