Stannous chloride dihydrate → HCID 60208811, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of Example 278A (2 g, 10.35 mmol) in ethyl acetate (60 ml) added tin(II) chloride dihydrate (8.18 g, 36.2 mmol), and the mixture was heated at 65° C. overnight. The reaction mixture was cooled to room temperature, diluted with 100 mL ethyl acetate, and 1M aqueous Na2CO3 was added until precipitation stopped. The solid was filtered through a pad of diatomaceous earth. The filter pad was suspended in ethyl acetate, stirred for a few minutes, and rinsed with ethyl acetate. The filtrate was washed with saturated aqueous Na2CO3, water, and brine, dried over MgSO4, filtered, and concentrated. Chromatography was performed with an Analogix 280 with an SF 40-80 column, 0% to 5% methanol/dichloromethane gradient over 30 minutes to provide the title compound. MS (DCI+) m/z 164.1 (M+H)+.

Provenance & Evidence