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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 2203701Generated: October 31, 2026

Dichloromethane → (3R,4R)-1-Boc-4-fluoro-3-piperidinol

https://huagongshe.com/reaction/2203701

Reaction equation

Participants

RoleNameHCIDCharge
ReactantDichloromethaneHCID 6344—
ReactantN,N-Diethylethanamine trihydrofluorideHCID 175505—
ReactantSodium BicarbonateHCID 516892—
Reactanttert-Butyl 7-Oxa-3-azabicyclo(4.1.0)heptane-3-carboxylateHCID 21991116—
Solvent1,2-DichloroethaneHCID 11—
Product(3R,4R)-1-Boc-4-fluoro-3-piperidinolHCID 6708693458.3%

Reaction Conditions

Temperature80 °C

Reaction Steps

A mixture of tert-butyl 7-oxa-3-azabicyclo[4.1.0]heptane-3-carboxylate (5.46 g, 27.4 mmol) and triethylamine trihydrofluoride (4.42 g, 27.4 mmol) in DCE (4 mL) was stirred at 80° C. (bath) for 18 hours. After cooling to room temperature, saturated sodium bicarbonate (20 mL) and DCM (30 mL) were added. The organic phase was separated, washed with brine, dried (sodium sulfate) and concentrated in vacuo. The residue obtained was purified by flash chromatography on silica gel (hexane:ethyl acetate 1:1) to give trans-tert-butyl 4-fluoro-3-hydroxypiperidine-1-carboxylate (3.5 g, 58%) as a solid.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS09365568B2
Source datasetuspto-grants-2016_06
ORD IDord-cb723baf04fd491eb4db68a963cdf3d2
Source noteuspto-grants-2016_06