(R)-(+)-4-氟-ALPHA-甲基苄醇

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

实验步骤: To a cooled solution (−15° C.) of the product of Step 1 (23.5 g, 0.168 mol) in toluene (300 ml) was added diphenylphosporyl azide (55.4 g, 0.395 mol) followed by DBU (30.4 ml, 0.2 mol). After stirring overnight, the resulting biphasic solution was poured into 500 ml 1 N HCl. The aqueous layer was extracted with toluene and the combined organic layers were washed with water, 1 N HCl and dried over Na2SO4. After removal of solvent, 25 g of crude product was obtained and was carried on to next step without further purification. The aqueous layer was extracted with toluene the combined organic layers were washed with water, 1 N HCl dried over Na2SO4 After removal of solvent

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

实验步骤: To a cooled solution (−15° C.) of the product of Step 1 (23.5 g, 0.168 mol) in toluene (300 ml) was added diphenylphosporyl azide (55.4 g, 0.395 mol) followed by DBU (30.4 ml, 0.2 mol). After stirring overnight, the resulting biphasic solution was poured into 500 ml 1 N HCl. The aqueous layer was extracted with toluene and the combined organic layers were washed with water, 1 N HCl and dried over Na2SO4. After removal of solvent, 25 g of crude product was obtained and was carried on to next step without further purification. The aqueous layer was extracted with toluene the combined organic layers were washed with water, 1 N HCl dried over Na2SO4 After removal of solvent

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

实验步骤: Starting with 4-(2,4-difluorophenyl)-N-{3-[(methylsulfonyl)methyl]phenyl}-1,3,5-triazin-2-amine (50 mg; 0.129 mmol), intermediate 42.1, and (R)-4-fluoro-α-methylbenzyl alcohol (74.4 mg; 0.515 mmol), example 67 was prepared analogously to the procedure for the preparation of example 42. was prepared analogously to the procedure for the preparation of example 42

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

实验步骤: To a cooled solution (−15° C.) of the product of Step 1 (23.5 g, 0.168 mol) in toluene (300 ml) was added diphenylphosporyl azide (55.4 g, 0.395 mol) followed by DBU (30.4 ml, 0.2 mol). After stirring overnight, the resulting biphasic solution was poured into 500 ml 1 N HCl. The aqueous layer was extracted with toluene and the combined organic layers were washed with water, 1 N HCl and dried over Na2SO4. After removal of solvent, 25 g of crude product was obtained and was carried on to next step without further purification. The aqueous layer was extracted with toluene the combined organic layers were washed with water, 1 N HCl dried over Na2SO4 After removal of solvent