反应详情

To prepare the compound of formula (Im), wherein R11 is chloro and m is 2, TFA (32 μl, 0.41 mmol) was added to an ice-cooled mixture of 4-chloro-N-(methoxymethyl)-N-[(trimethylsilyl)methyl]benzeneethanamine (1.5 g, 5.25 mmol) (Preparation 14) and N-(3,5-dichlorophenyl)succinimide (1 g, 4.13 mmol, prepared according to Fujinami et al., Agr. Biol. Chem. [1972], p. 318, incorporated herein by reference) in methylene chloride (10 mL). The reaction mixture was allowed to warm to RT over 3 h. The solution was washed with ammonium hydroxide. The organic layer was dried over MgSO4 and concentrated in vacuo to afford after chromatography over silica gel (CH2Cl2) the above-referenced compound as a white solid (1.56 g). Mp=115° C. 1H NMR (CDCl3): 7.40 (1H, br s), 7.15-7.35 (4H, m), 7.07 (2H, d, J=8.3 Hz), 3.4-3.5 (2H, m), 3.3-3.4 (2H, m), 2.55-2.8 (4H, m), 2.35-2.5 (2H, m).

1. customTo prepare the compound of formula (Im), wherein R11
2. temperaturecooled
3. customprepared
4. washThe solution was washed with ammonium hydroxide
5. dry with materialThe organic layer was dried over MgSO4
6. concentrationconcentrated in vacuo