Chlorosulfonic acid → HCID 11178065, compound

HRID 429137Notes

Reaction equation

HRID 429137 reaction equation
[Cl:1][C:2]([Cl:20])([Cl:19])[C:3]([N:5]1[CH2:10][CH2:9][N:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[O:17][CH3:18])[CH2:7][CH2:6]1)=[O:4].[Cl:21][S:22](O)(=[O:24])=[O:23]>ClCCl>[Cl:20][C:2]([Cl:1])([Cl:19])[C:3]([N:5]1[CH2:6][CH2:7][N:8]([C:11]2[CH:16]=[C:15]([S:22]([Cl:21])(=[O:24])=[O:23])[CH:14]=[CH:13][C:12]=2[O:17][CH3:18])[CH2:9][CH2:10]1)=[O:4]

Participants

4

Reactant 2

HCID 24638Chlorosulfonic acidHCID 33831142-(4-Trichloroacetylpiperazin-1-yl) anisole

Product 1

HCID 11178065HCID 11178065, compoundYield 46%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent2×

Procedure

A solution of 2-(4-trichloroacetylpiperazin-1-yl) anisole (D3) (10 g) in dichloromethane (115 ml) was added over 0.3 h to ice-cooled chlorosulfonic acid (52 ml). After 0.5 h at 0° C. then 1 h at ambient temperature, the solution was poured onto a mixture of ice-water (500 g) and dichloromethane (500 ml) with rapid stirring. The layers were separated and the organic phase was washed with water (2×800 ml), dried (MgSO4) and concentrated to give the title compound (D4) as a foam (6.0 g, 46%). MH+ 435/437.

Workup

  1. customThe layers were separated
  2. washthe organic phase was washed with water (2×800 ml)
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated

Sources & evidence

ORD record
ord-5daaafa129d144609c02ea75f6754f81
Source dataset
uspto-grants-2001_11
Patent number
US06316450B1

Reaction notes

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