1,2-Dichloroethane → HCID 57448175, compound

Participants

Reaction Steps

To 2B (6.30 g, 26.2 mmol) in DMF (52.5 mL) was added HOBT.H2O (4.9 g, 32.0 mmol) and EDC (5.98 g, 31.3 mmol). After stirring 1 h at rt, the reaction was cooled to 0° C. and 25% ammonium hydroxide was added. The reaction was stirred for 1.5 h and was then diluted with ethyl acetate/THF and washed with 1N HCl (2×) and 1 N NaOH (2×). The aqueous layer was back-extracted with ethyl acetate. The combined organic layers were washed with brine, dried (MgSO4), filtered and concentrated to provide 2C (5 g) as a yellow solid. LC-MS: 240.08 (M+H)+.

Provenance & Evidence