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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1087387Generated: November 1, 2026

Diethyl Ether → HCID 15661021, compound

https://huagongshe.com/reaction/1087387

Reaction equation

Participants

RoleNameHCIDCharge
ReactantDiethyl EtherHCID 3283—
ReactantAmmonium ChlorideHCID 25517—
ReactantHCID 9795017HCID 9795017—
ReactantHCID 178418348HCID 178418348—
SolventTetrahydrofuranHCID 8028—
ProductHCID 15661021HCID 15661021—

Reaction Conditions

Temperature0 °C

Reaction Steps

To a solution of dibenzo[b,f]thiepin-3-carboxylic acid (U.S. Pat. No. 4,536,507 (1985)) (415 mg, 1.63 mmole) in THF (20 mL) at 0° C. there was added methyl lithium in ether 1.4M (2.56 mL, 3.59 mmol); the mixture was stirred at 0° C. for 1 hour, then poured onto a well-stirred saturated aqueous ammonium chloride solution (100 mL). The organic phase was collected, washed twice with brine, dried and evaporated. Column chromatography on silica gel, eluting with a 1:2 mixture of ethyl acetate-hexane, afforded the title compound as a yellow solid (320 mg), m.p.: 82°-84° C.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS05036067
Source datasetuspto-grants-1991_07
ORD IDord-78670556aeed4019812c485d5d663bfb
Source noteuspto-grants-1991_07