Phosphorus oxychloride → 4-Chloro-5-iodo-6-methylpyrimidine

반응식

O[C:2]1[C:7]([I:8])=[C:6]([CH3:9])[N:5]=[CH:4][N:3]=1.O=P(Cl)(Cl)[Cl:12]>>[Cl:12][C:2]1[C:7]([I:8])=[C:6]([CH3:9])[N:5]=[CH:4][N:3]=1

참가 물질

반응물 2

HCID 24813Phosphorus oxychloride

HCID 1784332135-iodo-6-methyl-1H-pyrimidin-4-one

생성물 1

HCID 127953694-Chloro-5-iodo-6-methylpyrimidine

반응 조건

온도: 90 °C

실험 절차

A suspension of 90 g (0.38 mol) 4-hydroxy-5-iodo-6-methylpyrimidine in 600 mL POCl3 is heated for 1 h at 90° C. The reaction mixture is concentrated under reduced pressure and the residue is poured into crushed ice. The precipitated solid is collected by filtration and washed with water. After drying, the desired product is obtained as a solid (90 g; 93%).

후처리

concentrationThe reaction mixture is concentrated under reduced pressure
additionthe residue is poured
custominto crushed ice
filtrationThe precipitated solid is collected by filtration
washwashed with water
customAfter drying

출처 및 근거

ORD 기록: ord-434e92dce0cc4bbd838a2c387c442456
출처 데이터셋: uspto-grants-2016_04
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US09321771B2

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