Back
HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 471767Generated: October 31, 2026

Ethanol → HCID 67401491, compound

https://huagongshe.com/reaction/471767

Reaction equation

Participants

RoleNameHCIDCharge
ReactantEthanolHCID 702—
ReactantSodium HydroxideHCID 14798—
ReactantChlorosulfamic acidHCID 24499—
ReactantHCID 66746534HCID 66746534—
SolventEthyl AcetateHCID 8857—
SolventDimethylacetamideHCID 31374—
ProductHCID 67401491HCID 6740149178%

Reaction Steps

To a solution of 2-amino-6-(trans-2-methylcyclopentyloxy)benzonitrile (Example 264a) (150 mg, 0.694 mmol) in dimethylacetamide (3 mL) under N2 was added sulfamoyl chloride (3 equiv.). The reaction mixture was stirred at room temperature under N2 for 2 hours, diluted with ethyl acetate (50 mL) and quenched with water (20 mL). The layers were separated. The organic extract was evaporated. Ethanol (3 mL) and aqueous NaOH (2N, 2.5 equiv.) were consecutively added to the residue. The resulting mixture was heated at 90° C. for 16 hours. The workup was performed as in Example 111 to provide the desired product (160 mg, 78%) as a white powder. 1H NMR (400 MHz, DMSO-d6) δ 1.02 (d, J=6.4 Hz, 3H), 1.26 (m, 1H), 1.71 (br s, 3H), 1.89 (m, 1H), 2.12 (m, 1H), 2.24 (m, 1H), 4.55 (br s, 1H), 6.60 (d, J=8.0 Hz, 1H), 6.71 (d, J=8.0 Hz, 1H), 7.45 (t, J=8.0 Hz, 1H), 7.73 (br s, 1H), 8.35 (br s, 1H), 10.96 (br s, 1H). MS 296 (MH+).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08633186B2
Source datasetuspto-grants-2014_01
ORD IDord-20f77dfaf499417283ca67e2de4a6185
Source noteuspto-grants-2014_01