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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 2301021Generated: October 28, 2026

Ammonium Chloride → HCID 11419637, compound

https://huagongshe.com/reaction/2301021

Reaction equation

Participants

RoleNameHCIDCharge
ReactantAmmonium ChlorideHCID 25517—
ReactantSodium methanethiolateHCID 4378561—
ReactantHCID 54162932HCID 54162932—
SolventN-methyl-2-pyrrolidoneHCID 13387—
ProductHCID 11419637HCID 1141963762.5%

Reaction Conditions

Temperature120 °C

Reaction Steps

Sodium methanethiolate (49.5 mg) was added to a solution of (R)-N-[2-chloro-4-(2-fluorophenylsulphonyl)phenyl]-2-hydroxy-2-methyl-3,3,3-trifluoropropanamide (Method 63) (0.15 g) in NMP (1.5 ml) and the mixture was heated at 120° C. for 18 hours then cooled. Saturated aqueous ammonium chloride solution (15 ml) was added and the mixture was extracted with ethyl acetate (2×50 ml). The organic extracts were combined, washed with brine and dried. Volatile material was removed by evaporation and the residue was purified by chromatography on a silica gel Mega Bond Elut column eluting with 0-20% ethyl acetate/hexane to give the title compound (0.10 g) as a solid. NMR: (CDCl3): 1.75 (s, 3H), 2.4 (s, 3H), 3.6 (brs, 1H), 7.3 (t, 1H), 7.35 (t, 1H), 7.55 (m, 1H), 7.9 (dd, 1H), 8.05 (d, 1H), 8.25 (dd, 1H), 8.6 (d, 1H), 9.25 (brs, 1H); MS (ESP−): 452.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS06498275B1
Source datasetuspto-grants-2002_12
ORD IDord-f861349da4e9432b99270bc50d139764
Source noteuspto-grants-2002_12