Chlorosulfonic acid → 3-methoxythiophene-2-sulfonyl Chloride

温度

0 °C

Chlorosulfonic acid (ClSO3H, 2.31 g, 19.62 mmol) was slowly added at 0° C. to a solution of 3-methoxythiophene (2.29 g, 19.62 mmol) in CHCl3 (80 ml) The resulting mixture was stirred at 0° C. for 30 min. The solvent was evaporated under reduced pressure, at room temperature, the residue was suspended in POCl3 (15 ml, 156.96 mmol), and PCl5 (8.2 g, 39.24 mmol) was added slowly. The reaction was stirred at 60° C. for 18 h, then cooled to room temperature and poured onto crushed ice (200 g). The aqueous mixture was extracted with CHCl3 (2×150 ml) and the combined organic layers was dried (MgSO4). The solid was removed by filtration and the filtrate was concentrated to give 3-methoxy-2-thiophenesulfonyl chloride as a brown oil (1.81 g, 43% yield).

1. customThe solvent was evaporated under reduced pressure, at room temperature
2. stirringThe reaction was stirred at 60° C. for 18 h
3. temperaturecooled to room temperature
4. additionpoured
5. extractionThe aqueous mixture was extracted with CHCl3 (2×150 ml)
6. dry with materialthe combined organic layers was dried (MgSO4)
7. customThe solid was removed by filtration
8. concentrationthe filtrate was concentrated

ORDレコード

ord-260f0f7ab5354dafbb23a5e3d06e44bd

出典データセット

uspto-grants-1997_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05591761