Chlorosulfonic acid → HCID 11231761, compound

HRID 2215094Notes

Reaction equation

HRID 2215094 reaction equation
Cl[S:2](O)(=O)=O.[CH3:6][O:7][C:8](=[O:24])[CH:9]([CH:14]1[CH2:23][CH2:22][C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[O:15]1)[C:10]([O:12][CH3:13])=[O:11]>>[CH3:13][O:12][C:10](=[O:11])[CH:9]([CH:14]1[CH2:23][CH2:22][C:21]2[C:16](=[CH:17][CH:18]=[C:19]([SH:2])[CH:20]=2)[O:15]1)[C:8]([O:7][CH3:6])=[O:24]

Participants

3

Reactant 2

HCID 24638Chlorosulfonic acidHCID 11380043HCID 11380043, compound

Product 1

HCID 11231761HCID 11231761, compoundYield 53%

Procedure

Chlorosulfonic acid (15 mL) was cooled to 0° C. Then compound 5B (5.5 g. 20.8 mmol) was added over 30 min. The mixture was stirred at RT for 3 h and was poured into ice (100 g). The cloudy solution was extracted with ether (2×100 mL). The extracts were dried with magnesium sulfate and concentrated to give the desired product (4.0 g, 53%) as a yellow oil. The crude product was used immediately for the next step without purification.

Workup

  1. extractionThe cloudy solution was extracted with ether (2×100 mL)
  2. dry with materialThe extracts were dried with magnesium sulfate
  3. concentrationconcentrated

Sources & evidence

ORD record
ord-bff9250ae4c240ad8c430db3924b05cf
Source dataset
uspto-grants-2006_09
Patent number
US07109222B2

Reaction notes

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