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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 507084Generated: November 3, 2026

Methanol → HCID 11657467, compound

https://huagongshe.com/reaction/507084

Reaction equation

Participants

RoleNameHCIDCharge
ReactantMethanolHCID 887—
ReactantTriphenylphosphineHCID 11776—
Reactantethyl N-ethoxycarbonyliminocarbamateHCID 220568—
ReactantHCID 178427867HCID 178427867—
SolventDichloromethaneHCID 6344—
ProductHCID 11657467HCID 1165746753%

Reaction Steps

To a solution of (+/−)-isopropyl 5-[(3,5-bistrifluoromethyl-benzyl)-(1H-tetrazol-5-yl)-amino]-9-methyl-8-trifluormethyl-2,3,4,5-tetrahydrobenzo[b]azepine-1-carboxylate (87 mg, 0.139 mmol), methanol (0.564 mL, 13.9 mmol), triphenyl phosphine (73 mg, 0.278 mmol) in dry dichloromethane (3.4 mL) at 0° C., under nitrogen, add diethyl azodicarboxylate (0.128 mL, 0.278 mmol). Stir the reaction mixture at room temperature for 3 h. Remove the solvents under reduced pressure and purify the residue by flash chromatography, eluting with hexanes/ethyl acetate to afford the title compound (47 mg, 53%). MS (ES+): 639 (M+H).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS07786108B2
Source datasetuspto-grants-2010_08
ORD IDord-e45cdfff448741bfa1690679a9a7ac12
Source noteuspto-grants-2010_08