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

HRID 2387806

반응식

HRID 2387806 반응식
[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

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 178497678HCID 178497678, 화합물

생성물 1

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

반응 조건

온도
100 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-52557ab00a744435ab3b8ecf0242291e
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08268990B2

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