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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 245015Generated: October 29, 2026

Methylamine → HCID 86609861, compound

https://huagongshe.com/reaction/245015

Reaction equation

Participants

RoleNameHCIDCharge
ReactantMethylamineHCID 6329—
ReactantHCID 86609862HCID 86609862—
SolventTetrahydrofuranHCID 8028—
ProductHCID 86609861HCID 8660986182%

Reaction Conditions

Temperature-78 °C

Reaction Steps

Methylamine (0.5 ml) was bubbled into a mixture of Methanesulfonic acid 4-[7-(4-cyano-3-trifluoromethylphenyl)-8-oxo-6-thioxo-5,7-diazaspiro[3.4]oct-5-yl]phenylmethyl ester (50a) (0.059 g, 0.115 mmol) in THF (3 ml) cooled to −78° C. After 1 hour of reaction at −78° C., the mixture was concentrated and chromatographed (dichloromethane:acetone, 95:5; methanol) to yield 4-[5-(4-methylaminomethylphenyl)-8-oxo-6-thioxo-5,7-diazaspiro[3.4]oct-7-yl]-2-trifluoromethylbenzonitrile (50b) [RD155] (0.042 g, 0.095 mmol, 82%), the structure of which is illustrated in Formula 23, as a white powder.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08658681B2
Source datasetuspto-grants-2014_02
ORD IDord-3a8fe73a73d946329a827ea234e707d4
Source noteuspto-grants-2014_02