Phosphorus oxychloride → HCID 58368608、化合物

反応式

[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

参加物

反応物 2

HCID 24813Phosphorus oxychloride

HCID 822385HCID 822385、化合物

生成物 1

HCID 58368608HCID 58368608、化合物

反応条件

温度: 70 °C

実験手順

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.

後処理

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%)

出典と根拠

ORDレコード: ord-6f0e3142aefd4175b2a8ae550eb374c3
出典データセット: uspto-grants-2014_03
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US08680108B2

反応ノート

読み込み中…

参加物