反应详情

To a solution of 5-(2,6-dichloro-4-nitro-phenoxy)-2-methoxy-N-nonyl-benzamide (173 mg, 0.36 mmol) in CH2Cl2 (3 ml) was added a solution of BBr3 (0.72 ml of a 1 M solution in CH2Cl2). The resulting mixture was stirred at RT for 1.5 h then quenched by addition of MeOH (1 ml) and water (10 ml). The resulting mixture was stirred at RT for 30 min then further diluted with 1 M HCl (10 ml) and extracted with CH2Cl2 (3×5 ml). The combined CH2Cl2 extracts were washed with brine, dried over Na2SO4, filtered and concentrated to give the title compound of Step D (168 mg) as a viscous oil. The title product of Step D was used in the next step without further purification. MS (APCl−) Calc.: 468.1, Found: 467.2 (M−1).

1. customthen quenched by addition of MeOH (1 ml) and water (10 ml)
2. stirringThe resulting mixture was stirred at RT for 30 min
3. additionthen further diluted with 1 M HCl (10 ml)
4. extractionextracted with CH2Cl2 (3×5 ml)
5. washThe combined CH2Cl2 extracts were washed with brine
6. dry with materialdried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated