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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1015977Generated: October 31, 2026

Triethylamine → 1,1-Dimethylethyl (9S)-9-[[(phenylmethoxy)carbonyl]amino]-1-oxa-7-azaspiro[4.4]nonane-7-carboxylate

https://huagongshe.com/reaction/1015977

Reaction equation

Participants

RoleNameHCIDCharge
ReactantTriethylamineHCID 8471—
ReactantMethanesulfonyl chlorideHCID 31297—
ReactantHCID 59556045HCID 59556045—
SolventDichloromethaneHCID 6344—
Product1,1-Dimethylethyl (9S)-9-[[(phenylmethoxy)carbonyl]amino]-1-oxa-7-azaspiro[4.4]nonane-7-carboxylateHCID 5955605541.9%

Reaction Conditions

Temperature60 °C

Reaction Steps

To a solution of 0.80 g of the diol of step D in 15 mL of dichloromethane at 0° C. were added 0.2 mL of methanesulfonyl chloride and 0.8 mL of triethylamine. After being stirred for 1 hour, the mixture was refluxed at 60° C. overnight. Solvent was removed under vacuum. The residue was taken up in EtOAc/water and the two phases were separated. The water phase was extracted with EtOAc twice. The combined organic was dried over Na2SO4. Solvent was removed under vacuum. Column chromatography on silica gel using 15% EtOAc/hexane to 100% EtOAc as eluent provided 0.32 g of the title compound. MS (M+H)+ 377.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS07985730B2
Source datasetuspto-grants-2011_07
ORD IDord-69d2e27978254ab48fa5816a38edf72f
Source noteuspto-grants-2011_07