反应详情

To a solution of 2-[4-[2-amino-3-(4-fluorophenyl)-propionyl]-3-cyclopropylmethyl-2-oxo-piperazin-1-yl}-N-methyl-3-naphthalen-2-yl-propionamide, 18, (100 mg, 0.155 mmol) and triethylamine (20 mg, 0.2 mmole) in CH2Cl2 (5 mL) at 0° C. is added dropwise acetyl chloride (13.4 mg, 0.17 mmole). The reaction is allowed to warm to room temperature and stirred 1 hour. The reaction is diluted with CH2Cl2 (10 mL) and extracted with water then brine, dried and concentrated in vacuo to afford a residue which is purified over silica gel to afford the desired product. 13C NMR (CDCl3, 75 MHz), 170.12, 169.90, 169.82, 169.49, 169.35, 167.70, 134.07, 133.67, 132.57, 131.64, 128.65, 127.83, 127.80, 127.70, 127.51, 127.23, 127.15, 126.64, 126.15, 115.87, 115.79, 115.60, 115.51, 58.65, 57.40, 56.61, 56.43, 50.61, 50.09, 42.76, 41.96, 41.55, 39.84, 38.39, 37.77, 36.89, 34.65, 34.09, 26.59, 23.26, 23.07, 7.20, 7.12, 4.83, 4.69, 4.45; MS, (ES-MS) m/z 573 (M+1).

1. extractionextracted with water
2. dry with materialbrine, dried
3. concentrationconcentrated in vacuo
4. customto afford a residue which
5. customis purified over silica gel