反应详情

To dimethylamine hydrochloride (26.1 mg) in toluene (2 mL) was added Al(CH3)3 (0.16 mL) at 0° C. The reaction stirred for about 30 minutes before adding the product of EXAMPLE 91 (85 mg) in toluene (1 mL). The reaction stirred for 3.5 hours at 50° C. and was quenched with aqueous 1 M HCl. The reaction was diluted with EtOAc washed with aqueous 1 M HCl. The solution was dried (Na2SO4) and concentrated. The concentrated residue was purified by preparative TLC on silica gel eluted with 6% methanol in CH2Cl2 affording the title compound. HPLC/MS: 543.0 (M+1), 545.0 (M+3); Rt=3.51 min.

1. stirringThe reaction stirred for 3.5 hours at 50° C.
2. customwas quenched with aqueous 1 M HCl
3. additionThe reaction was diluted with EtOAc
4. washwashed with aqueous 1 M HCl
5. dry with materialThe solution was dried (Na2SO4)
6. concentrationconcentrated
7. customThe concentrated residue was purified by preparative TLC on silica gel
8. washeluted with 6% methanol in CH2Cl2 affording the title compound