反应详情

A mixture of 4-(3-thienylmethoxy)-2-[2-(trimethylsilyl)ethoxy]methoxybenzoic acid (3.09 g), methyl aminoacetate hydrochloride (0.99 g), 1-hydroxybenzotriazole (1.28 g), triethylamine (0.8 g) and dimethylformamide (50 mL) is stirred at ambient temperature for 16 hours. It is then concentrated in vacuo and the resulting residue is dissolved in ethyl acetate (100 mL), washed quickly with hydrochloric acid (2×50 mL; 1 N), and then washed with saturated aqueous sodium bicarbonate solution (50 mL) and with water (50 mL), then dried over magnesium sulphate, filtered and concentrated in vacuo, to give 1-[N-(methoxycarbonylmethyl)carbamoyl]-4-(3-thienylmethoxy)-2-[2-(trimethylsilyl)ethoxy]methoxybenzene, in the form of a yellow oil.

1. concentrationIt is then concentrated in vacuo
2. dissolutionthe resulting residue is dissolved in ethyl acetate (100 mL)
3. washwashed quickly with hydrochloric acid (2×50 mL; 1 N)
4. washwashed with saturated aqueous sodium bicarbonate solution (50 mL) and with water (50 mL)
5. dry with materialdried over magnesium sulphate
6. filtrationfiltered
7. concentrationconcentrated in vacuo