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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 264021Generated: October 30, 2026

Methanol → 4-(2,4-Dioxo-8-methyl-1,3,8-triazaspiro[4.5]-decan-3-yl)-2-(trifluoromethyl)-benzonitrile

https://huagongshe.com/reaction/264021

Reaction equation

Participants

RoleNameHCIDCharge
ReactantMethanolHCID 887—
ReactantSodium ChlorideHCID 5234—
ReactantAmmonium HydroxideHCID 14923—
ReactantHCID 21846478HCID 21846478—
SolventEthyl AcetateHCID 8857—
Product4-(2,4-Dioxo-8-methyl-1,3,8-triazaspiro[4.5]-decan-3-yl)-2-(trifluoromethyl)-benzonitrileHCID 21846487—

Reaction Steps

Using the procedure of Example 2, 3 g of the product of Example 22, 70 ml of methanol and 17 ml of 2N hydrochloric were reacted and the solution was refluxed for 90 minutes. It was poured into 200 ml of ammonium hydroxide +100 g of ice saturated with sodium chloride and extraction was carried out 4 times with ethyl acetate. The extracts were washed with salt water, dried and purified on silica with methylene chloride-methanol: 9-1 as eluant. After crystallization from methylene chloride-isopropyl ether, 2.12 g of the expected product (white crystals) melting at 188°-189° C were obtained.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS05646172
Source datasetuspto-grants-1997_07
ORD IDord-d44bbc50282a497da1673d545a076bb2
Source noteuspto-grants-1997_07