Hydrochloric Acid → HCID 66727499, compound

HRID 2198233Notes

Reaction equation

HRID 2198233 reaction equation
[CH3:1][S:2]([C:5]1[CH:10]=[C:9]([C@@H:11]([NH:13]S(C(C)(C)C)=O)[CH3:12])[CH:8]=[CH:7][N:6]=1)(=[O:4])=[O:3].[ClH:20].O1CCOCC1>CO>[ClH:20].[CH3:1][S:2]([C:5]1[CH:10]=[C:9]([C@@H:11]([NH2:13])[CH3:12])[CH:8]=[CH:7][N:6]=1)(=[O:4])=[O:3]

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 66727614HCID 66727614, compound

Product 1

HCID 66727499HCID 66727499, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To a solution of 2-methyl-propane-2-sulfinic acid [(S)-1-(2-methanesulfonyl-pyridin-4-yl)-ethyl]-amide (29.9 g, 98.2 mmol) in methanol (160 mL) was added a solution of 4 N HCl in dioxane (25.8 mL, 103 mmol). After 1 hour, the solution was concentrated to half the original volume and diluted with toluene (100 mL), and concentrated. The crude material was diluted with toluene (3×100 mL) and concentrated in vacuo and dried in vacuo for 18 hours to afford the title compound as an off-white solid which was used without further purification.

Workup

  1. concentrationthe solution was concentrated to half the original volume
  2. additiondiluted with toluene (100 mL)
  3. concentrationconcentrated
  4. additionThe crude material was diluted with toluene (3×100 mL)
  5. concentrationconcentrated in vacuo
  6. customdried in vacuo for 18 hours

Sources & evidence

ORD record
ord-d3fd9e47c579493e92dc073cb36747b0
Source dataset
uspto-grants-2012_12
Patent number
US08338610B2

Reaction notes

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