6-Methoxy-3-trichloromethyl-3H-isobenzofuran-1-one synthesis
- Product Name:6-Methoxy-3-trichloromethyl-3H-isobenzofuran-1-one
- CAS Number:82735-28-2
- Molecular formula:C10H7Cl3O3
- Molecular Weight:281.52
Yield:82735-28-2 97%
Reaction Conditions:
with sulfuric acid at 20; for 12 h;
Steps:
1. 3-Trichloromethyl-6-methoxy-1(3H)-isobenzofuranone (1)
3-Methoxylbenzonic acid (3.1g, 20.4mmol) was dissolved in concentrated sulfuric acid (9.3mL) and chloral hydrate (3.72g, 22.5mmol) was added. After reacting for 12 h at room temperature, the mixture was poured onto ice (30g), and the precipitated product was collected by filtration, washed with saturated sodium bicarbonate solution to pH=7, and air-dried to give compound 1 as white solid(5.6g, 97.0%). mp 128-130oC (ref: 132-134oC)14; MS (ESI, m/z): 280[M]+
References:
Tang, Zhichao;Niu, Shaoxiong;Liu, Fei;Lao, Kejing;Miao, Jingshan;Ji, Jinzi;Wang, Xiang;Yan, Ming;Zhang, Luyong;You, Qidong;Xiao, Hong;Xiang, Hua [Bioorganic and Medicinal Chemistry Letters,2014,vol. 24,# 9,p. 2129 - 2133] Location in patent:supporting information
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