4-chlorobutane-1-sulphonyl chloride synthesis

11synthesis methods

Product Name:4-chlorobutane-1-sulphonyl chloride
CAS Number:1633-84-7
Molecular formula:C4H8Cl2O2S
Molecular Weight:191.08

1633-83-6 Synthesis

1633-83-6
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$17.00/5g

1633-84-7
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$23.00/100mg

Yield: 90%

Reaction Conditions:

with thionyl chloride in DMF (N,N-dimethyl-formamide) at 70; for 72 h;

Steps:

20 Description 20; 4-CHLORO-1-BUTANESULFONYL CHLORIDE (D20)
To a mixture of [1,2] oxathiane 2,2-dioxide (D23) (50 g, 367 mmol, 1 equiv) and SOCS (29 ML, 401 mmol, 1.1 equiv) was added DMF (4 MI, 51.6 mmol, 0.14 equiv). The resulting mixture was stirred under nitrogen at 70 C for 3 days. A second portion of SOC12 (10 ml, 137 mmol, 0. 37 equiv) was added. The mixture was stirred at 70 C for another 3 days and then cooled to room temperature and concentrated in vacuo. The residue was diluted with toluene then concentrated in vacuo. This procedure was repeated and the residue was dried under vacuum for 16 h to give crude 4-CHLORO-1-BUTANESULFONYL chloride (D20) (63 g, 90%).

References:

GLAXO GROUP LIMITED WO2004/50619, 2004, A1 Location in patent:Page 23-24