2-溴-3-甲基苯甲酰基 氯化物

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 2-phenethylamine (0.28 mL, 2.195 mmol) in DCM (2.0 mL) was added 2-bromo-3-methylbenzoyl chloride (0.15 mL, 0.998 mmol) dropwise via syringe at ambient temperature. Mixture was allowed to stir overnight, then diluted with water (30 mL) and extracted with DCM (30 mL). The organic extract was washed with 1N HCl (2×25 mL) and 1N NaOH (2×25 mL) and dried over MgSO4. The solution was filtered and concentrated in vacuo to give 2-bromo-3-methyl-N-phenethylbenzamide as a white solid. extracted with DCM (30 mL) The organic extract was washed with 1N HCl (2×25 mL) and 1N NaOH (2×25 mL) dried over MgSO4 The solution was filtered concentrated in vacuo

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 2-phenethylamine (0.28 mL, 2.195 mmol) in DCM (2.0 mL) was added 2-bromo-3-methylbenzoyl chloride (0.15 mL, 0.998 mmol) dropwise via syringe at ambient temperature. Mixture was allowed to stir overnight, then diluted with water (30 mL) and extracted with DCM (30 mL). The organic extract was washed with 1N HCl (2×25 mL) and 1N NaOH (2×25 mL) and dried over MgSO4. The solution was filtered and concentrated in vacuo to give 2-bromo-3-methyl-N-phenethylbenzamide as a white solid. extracted with DCM (30 mL) The organic extract was washed with 1N HCl (2×25 mL) and 1N NaOH (2×25 mL) dried over MgSO4 The solution was filtered concentrated in vacuo

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A suspension of 2-bromo-3-methylbenzoic acid (2.07 g, 9.63 mmol) in DCM (48.1 mL) was cooled to 0° C. Oxalyl chloride (0.9 mL, 10.14 mmol) was added dropwise via syringe. After addition, the cooling bath was removed and the reaction mixture stirred overnight. The mixture was concentrated in vacuo to remove solvent and excess reagent, affording 2-bromo-3-methylbenzoyl chloride as a cloudy white oil. After addition the cooling bath was removed The mixture was concentrated in vacuo to remove solvent and excess reagent

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 2-phenethylamine (0.28 mL, 2.195 mmol) in DCM (2.0 mL) was added 2-bromo-3-methylbenzoyl chloride (0.15 mL, 0.998 mmol) dropwise via syringe at ambient temperature. Mixture was allowed to stir overnight, then diluted with water (30 mL) and extracted with DCM (30 mL). The organic extract was washed with 1N HCl (2×25 mL) and 1N NaOH (2×25 mL) and dried over MgSO4. The solution was filtered and concentrated in vacuo to give 2-bromo-3-methyl-N-phenethylbenzamide as a white solid. extracted with DCM (30 mL) The organic extract was washed with 1N HCl (2×25 mL) and 1N NaOH (2×25 mL) dried over MgSO4 The solution was filtered concentrated in vacuo

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A suspension of 2-bromo-3-methylbenzoic acid (2.07 g, 9.63 mmol) in DCM (48.1 mL) was cooled to 0° C. Oxalyl chloride (0.9 mL, 10.14 mmol) was added dropwise via syringe. After addition, the cooling bath was removed and the reaction mixture stirred overnight. The mixture was concentrated in vacuo to remove solvent and excess reagent, affording 2-bromo-3-methylbenzoyl chloride as a cloudy white oil. After addition the cooling bath was removed The mixture was concentrated in vacuo to remove solvent and excess reagent