Reaktion #676852

ord-fe9222313f924dadb315294cf65a9697

Reaktionsgleichung

Cc1c(S(=O)(=O)O)sc2ccc(F)cc12
5-fluoro-3-methylbenzothiophene-2-sulfonic acid
O=P(Cl)(Cl)Cl
POCl3
→
Cc1c(S(=O)(=O)Cl)sc2ccc(F)cc12
title compound
Ausbeute 93.0%
Cc1c(S(=O)(=O)Cl)sc2ccc(F)cc12
5-Fluoro-3-methyl-benzothiophene-2-sulfonyl chloride
Ausbeute 93.0%

Edukte

Cc1c(S(=O)(=O)O)sc2ccc(F)cc12
5-fluoro-3-methylbenzothiophene-2-sulfonic acid
O=P(Cl)(Cl)Cl
POCl3

Reagenzien

Keine

Reaktionsbedingungen

Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe POCl3 was evaporated
  2. 2
    workup.DISSOLUTIONthe crude product was dissolved in CH2Cl2
  3. 3
    Waschenwashed with water
  4. 4
    SonstigeThe organic phase was dried
  5. 5
    Sonstigeevaporated

Vorschrift

A mixture of 5-fluoro-3-methylbenzothiophene-2-sulfonic acid (230 mg, 0.93 mmol) in POCl3 (5 mL) was heated at 60° C. over night. The POCl3 was evaporated and the crude product was dissolved in CH2Cl2 and washed with water. The organic phase was dried and evaporated to give 0.23 g (93%) of the title compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09233946B2uspto-grants-2016_01