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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1670420Generated: November 3, 2026

Dichloromethane → HCID 57617721, compound

https://huagongshe.com/reaction/1670420

Reaction equation

Participants

RoleNameHCIDCharge
ReactantDichloromethaneHCID 6344—
Reactant3-Amino-5-phenyl-1,3-dihydro-1,4-benzodiazepin-2-oneHCID 4259649—
ReactantSodium 2-ethylhexanoateHCID 23672331—
ReactantHCID 57617720HCID 57617720—
SolventTetrahydrofuranHCID 8028—
ProductHCID 57617721HCID 57617721125.8%

Reaction Conditions

Temperature60 °C

Reaction Steps

235 mg of 2 (818 μmol), 400 mg of 14 (1.59 mmol), 340 mg of sodium 2-ethylhexanoate (2.04 mmol) in 3.5 mL of THF are successively introduced into a 30 mL round-bottomed flask, with stirring and under an argon atmosphere. The mixture is heated at 60° C. for 5 h and the stirring is maintained at RT for 24 h. 15 mL of CH2Cl2 are added to the reaction medium. The mixture is washed with twice 10 mL of HCl (1N) and then 10 mL of a saturated aqueous NaCl solution. The organic phase is dried over anhydrous magnesium sulphate, filtered and then evaporated to dryness. 510 mg of crude product are obtained, which product is chromatographed on a silica cartridge (30 g, eluent CH2Cl2/MeOH 97/3). 73 mg of expected product Ex6 are recovered.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS07994161B2
Source datasetuspto-grants-2011_08
ORD IDord-13062ea9d50742ccac4efa8fc18274e2
Source noteuspto-grants-2011_08