2-(1-(4-chlorophenylsulfonyl)vinyl)-1,4-difluorobenzene synthesis
- Product Name:2-(1-(4-chlorophenylsulfonyl)vinyl)-1,4-difluorobenzene
- CAS Number:471905-61-0
- Molecular formula:C14H9ClF2O2S
- Molecular Weight:314.73
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Yield:471905-61-0 95%
Reaction Conditions:
with bis-(dimethylamino)methane in DMF (N,N-dimethyl-formamide) at 60; for 5 h;
Steps:
3 Example 3; 2-[[(4-chlorophenyl)sulfonyl]ethenyl]-1,4-difluorobenzene
[2- [ [ (4-CHLOROPHENYL)] sulfonyl] [METHYL]-1,] 4-difluorobenzene (Example 2) [(100G,] 0. [33MOL)] and N, N, N', N'-tetramethyldiaminomethane (34.2g, 0. [50MOL)] were dissolved in dimethyl formamide (lOOOmL) at [60°C.] Acetic anhydride (68.3g, [L.] [OOMOL)] was added slowly and the reaction mixture was aged for 5 hours. Water (1000 mL) was added dropwise and the resulting slurry was cooled to [5°C.] The solids were filtered, and the cake washed sequentially with dimethyl formamide: water (40: 60,200mL) and water [(500ML).] Drying overnight in vacuo at [40°C] under a nitrogen stream furnished 2- [[1- [ (4-CHLOROPHENYL) SULFONYL] ETHENYL]-1,] 4-difluorobenzene (98g, 95%). [1H] NMR [(CDCL3)] 7.64-7. 59 (2H, m), 7.43-7. 39 (2H, [M),] 7.27-7. 22 [(1H,] m), 7.08-6. 88 (2H, [M),] 6.88 [(1H,] s) and 6.09 [(1H,] s).
References:
WO2004/13090,2004,A1 Location in patent:Page 12
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