Phosphorus oxychloride → HCID 58368608, 화합물

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[C:1]([C:4]1[NH:5][C:6](=O)[C:7]2[C:12]([C:13]=1[OH:14])=[CH:11][CH:10]=[CH:9][CH:8]=2)(=[O:3])[CH3:2].P(Cl)(Cl)([Cl:18])=O>>[Cl:18][C:6]1[C:7]2[C:12](=[CH:11][CH:10]=[CH:9][CH:8]=2)[C:13]([OH:14])=[C:4]([C:1](=[O:3])[CH3:2])[N:5]=1

참가 물질

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HCID 24813Phosphorus oxychloride

HCID 822385HCID 822385, 화합물

생성물 1

HCID 58368608HCID 58368608, 화합물

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온도: 70 °C

실험 절차

A mixture of 3-acetyl-4-hydroxyisoquinolin-1(2H)-one (10.0 g, 49.2 mmol) and phosphoryl chloride (45.87 mL) was heated at 70° C. for 24 hours. After cooling to room temperature, the mixture was poured onto crushed ice and stirred for 30 minutes. The precipitated solid was collected by filtration in vacuum and air dried (9.82 g, 90%). LCMS calculated for C11H9ClNO2 (M+H)+: m/z=222.0; Found: 222.1.

후처리

temperatureAfter cooling to room temperature
additionthe mixture was poured
customonto crushed ice
filtrationThe precipitated solid was collected by filtration in vacuum and air
customdried (9.82 g, 90%)

출처 및 근거

ORD 기록: ord-6f0e3142aefd4175b2a8ae550eb374c3
출처 데이터셋: uspto-grants-2014_03
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US08680108B2

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