Dichloromethane → 4,6-Dichloro-2-methylpyrimidine

반응식

O[C:2]1[CH:7]=C(O)[N:5]=[C:4]([CH3:9])[N:3]=1.P(Cl)(Cl)([Cl:12])=O.Cl[CH2:16][Cl:17]>>[Cl:12][C:2]1[CH:7]=[C:16]([Cl:17])[N:5]=[C:4]([CH3:9])[N:3]=1

참가 물질

반응물 3

HCID 6344Dichloromethane

HCID 24813Phosphorus oxychloride

HCID 178418389HCID 178418389, 화합물

생성물 1

HCID 2349974,6-Dichloro-2-methylpyrimidine

반응 조건

온도: 95 °C

실험 절차

4,6-Dihydroxy-2-methylpyrimidine 21 (1.03 g, 8.1 mmol) is suspended in 2.5 mL phosphorus oxychloride (27.3 mmol). The mixture is heated to 95° C. for 18 hours. Upon cooling, the mixture is diluted with dichloromethane (100 mL) and filtered. It is then washed with water, saturated aqueous sodium bicarbonate and brine, then concentrated to yield 4,6-dichloro-2-methylpyrimidine 22 as a white powder. 1H-NMR (400 MHz, CDCl3) δ=7.45 (s, 1H), 2.77 (s, 3H). MS calculated for C5H5Cl2N2 (M+H+) 162.99. found 163.2.

후처리

temperatureUpon cooling
filtrationfiltered
washIt is then washed with water, saturated aqueous sodium bicarbonate and brine
concentrationconcentrated

출처 및 근거

ORD 기록: ord-9f9d73ccab04499d925e69c5dfa51904
출처 데이터셋: uspto-grants-2010_06
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US07745445B2

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