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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1059417Generated: October 31, 2026

Ammonium Chloride → HCID 178496765, compound

https://huagongshe.com/reaction/1059417

Reaction equation

Participants

RoleNameHCIDCharge
ReactantAmmonium ChlorideHCID 25517—
ReactantTrimethylsilyldiazomethaneHCID 167693—
ReactantHCID 69884035HCID 69884035—
ReactantButyllithiumHCID 178418339—
SolventTetrahydrofuranHCID 8028—
SolventHexaneHCID 8058—
ProductHCID 178496765HCID 178496765—

Reaction Conditions

Temperature-78 °C

Reaction Steps

1.5 ml of a 2.0 M solution of (trimethylsilyl)-diazomethane in hexane was added to dry tetrahydrofuran (7 ml) in a nitrogen atmosphere and cooled to −78° C. After dropping 1.0 ml of a 1.6 M n-butyllithium solution in n-hexane thereinto, the resulting mixture was stirred for 30 minutes. Into the reaction mixture was dropped a solution of 410 mg of 8-(2-benzenesulfonylvinyl)-10-methoxymethyl-10H-pyrazino[2,3-b][1,4]benzothiazine obtained in Example 1080-1 in dry tetrahydrofuran (5 ml). Then the reaction mixture was gradually heated to room temperature and an aqueous solution of ammonium chloride was added thereto followed by extraction with ethyl acetate. Then the mixture was dried over anhydrous sodium sulfate. After distilling off the solvent under reduced pressure, the obtained residue was purified by silica gel column chromatography (eluted with ethyl acetate/n-hexane) to thereby give 130 mg of the title compound as yellow crystals.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS06518423B1
Source datasetuspto-grants-2003_02
ORD IDord-789996e5ada24296a4b68a9242b091ec
Source noteuspto-grants-2003_02