N,N-二乙基-1,1,2,3,3,3-六氟丙胺

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:25.01; pressure:0.00; stir:

反应条件: temp:25.01; pressure:0.00; stir:

反应条件: temp:25.01; pressure:0.00; stir:

反应条件: temp:25.01; pressure:0.00; stir:

反应条件: temp:25.01; pressure:0.00; stir:

反应条件: temp:25.01; pressure:0.00; stir:

反应条件: temp:25.01; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:22.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: (4R,5R)-3-dichloroacetyl-2,2-dimethyl-4-hydroxymethyl-5-[4-(methylsulfonyl)phenyl]-1,3-oxazolidine (Compound XIIa) (81 g, 0.2050 moles) in methylene chloride (450 ml) reacts with N,N-diethyl-1,1,2,3,3,3-hexafluoro-1-propanamine (Ishikawa Reagent) (73.2 g, 0.328 moles) at 95-105° C. for 2-4 hours. Cooling to 20-25° C., quenching with 25% aqueous sodium hydroxide and water (2000 mL) and separation of the methylene chloride layer gives a solution of (4S,5R)-3-dichloroacetyl-2,2-dimethyl-4-fluoromethyl-5-[4-(methylsulfonyl)phenyl]-1,3-oxazolidine (Compound XIIIa) for use as an intermediate for the next step in the process. quenching with 25% aqueous sodium hydroxide and water (2000 mL) and separation of the methylene chloride layer