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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1173190Generated: November 2, 2026

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

https://huagongshe.com/reaction/1173190

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 numberUS07834021B2
Source datasetuspto-grants-2010_11
ORD IDord-cad043e6b6404d6682852da2aa9f2b81
Source noteuspto-grants-2010_11