Trifluoromethylsulfonamide → HCID 57925961、化合物
反応式
[CH3:1][N:2]1[CH2:7][CH2:6][P:5]([C:9]2[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][CH:10]=2)(=[O:8])[CH2:4][CH2:3]1.[F:16][C:17]([F:23])([F:22])[S:18](N)(=[O:20])=[O:19]>CN(C=O)C>[F:16][C:17]([F:23])([F:22])[S:18]([O:15][C:12]1[CH:13]=[CH:14][C:9]([P:5]2(=[O:8])[CH2:6][CH2:7][N:2]([CH3:1])[CH2:3][CH2:4]2)=[CH:10][CH:11]=1)(=[O:20])=[O:19]参加物
4
実験手順
4-(1-Methyl-4-oxido-1,4-azaphosphinan-4-yl)phenol (0.50 g, 2.22 mmol) was made 0.5 M in DMF and N-Phenyl-bis(trifluorometanesulfonamide (1.19 g, 3.33 mmol) was added, followed by TEA (0.62 mL, 4.44 mmol). The mixture was stirred at ambient temperature for 16 h then the precipitate was filtered off and the filtrate was concentrated in vacuo. The residue was purified by HPLC (20-95% MeCN in water w/0.025% TFA). Pure fractions were identified, combined and concentrated in vacuo. The residue was taken up in EtOAc and washed with saturated aqueous sodium bicarbonate (1×) then dried (MgSO4) and concentrated in vacuo to afford the requisite product as a freebase. MS: cal'd 358 (MH+), exp 358 (MH