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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1431147Generated: November 3, 2026

Water → HCID 86662322, compound

https://huagongshe.com/reaction/1431147

Reaction equation

Participants

RoleNameHCIDCharge
ReactantWaterHCID 962—
ReactantHCID 86662323HCID 86662323—
SolventFormic AcidHCID 284—
SolventFormaldehydeHCID 712—
ProductHCID 86662322HCID 8666232261.9%

Reaction Conditions

Temperature70 °C

Reaction Steps

(1S,4S)-5-(6-Chloro-pyridin-3-ylmethyl)-2,5-diaza-bicyclo[2.2.1]heptane-2-carboxylic acid tert-butyl ester (1.1 g, 3.4 mmol) was dissolved in a mixture of 11.3 ml of formic acid and 22.6 ml of formalin. The reaction was heated at 70° C. for 4 hours, and then cooled to room temperature. Water was added and the aqueous layer was extracted with DCM. The aqueous layer was carefully basified with solid potassium carbonate and extracted 3 times with DCM. The crude product was purified by chromatography using a gradient of 5% to 25% methanol in DCM. Ammonium hydroxide (approximately 2%) had been added to the methanol. 500 mg of a colorless liquid was obtained (61.9%).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08940741B2
Source datasetuspto-grants-2015_01
ORD IDord-72c439d61aea40c8ada39e9b9643b740
Source noteuspto-grants-2015_01