Hydrochloric Acid → HCID 67181086, compound

HRID 2425560Notes

Reaction equation

HRID 2425560 reaction equation
[CH3:1][N:2]1[C:6]([C:7]([F:10])([F:9])[F:8])=[C:5]([C@H:11]([NH:13][S@@](C(C)(C)C)=O)[CH3:12])[CH:4]=[N:3]1.[ClH:20]>O1CCOCC1>[ClH:20].[ClH:20].[CH3:1][N:2]1[C:6]([C:7]([F:8])([F:9])[F:10])=[C:5]([C@H:11]([NH2:13])[CH3:12])[CH:4]=[N:3]1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 67183280HCID 67183280, compound

Product 1

HCID 67181086HCID 67181086, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Procedure

(R)-N-((R)-1-(1-methyl-5-(trifluoromethyl)-1H-pyrazol-4-yl)ethyl)-2-methylpropane-2-sulfinamide (0.135 g, 0.00045 mole) was dissolved in HCl in dioxane (4M, 8 ml) and the solution stirred at room temperature overnight under nitrogen. The solution was evaporated and the residue suspended in ether and the white solid filtered off under a blanket of nitrogen. Yield 120 mg 99% (hygroscopic). 1H NMR (400 MHz CD3OD) 7.74 (s, 1H) 4.67, 4.66, 4.64, 4.62 (q, 1H) 4.02 (s, 3H) 1.63, 1.61 (d, 3H) MS (ESI) m/z 194 (M+H)+177 (M+H—NH3)+TLC CH2Cl2:MeOH:NH4OH 95:5:0.5 0.2 UV−ve KMnO4+ve [α]D=+2.87° (c=2.003, CH3OH)

Workup

  1. customThe solution was evaporated
  2. filtrationthe white solid filtered off under a blanket of nitrogen

Sources & evidence

ORD record
ord-a2f84fc8adb34117b566d54013a13402
Source dataset
uspto-grants-2011_06
Patent number
US07964732B2

Reaction notes

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