Ammonium Acetate → N-(tert-Butyl)-2-amino-2-(4-fluorophenyl)ethanesulfonamide

HRID 72369

반응식

HRID 72369 반응식
[C:1]([NH:5][S:6]([CH2:9][C:10]([C:12]1[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=1)=O)(=[O:8])=[O:7])([CH3:4])([CH3:3])[CH3:2].C([O-])(=O)C.[NH4+].C([BH3-])#[N:25].[Na+]>CO>[C:1]([NH:5][S:6]([CH2:9][CH:10]([NH2:25])[C:12]1[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=1)(=[O:8])=[O:7])([CH3:4])([CH3:3])[CH3:2]

참가 물질

5

반응물 3

HCID 517165Ammonium AcetateHCID 5003444Sodium cyanoborohydrideHCID 68288463N-(tert-Butyl)-2-(4-fluorophenyl)-2-oxoethanesulfonamide

생성물 1

HCID 68287917N-(tert-Butyl)-2-amino-2-(4-fluorophenyl)ethanesulfonamide

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 0.66 g of N-(tert-butyl)-2-(4-fluorophenyl)-2-oxoethanesulfonamide, 1.85 g of ammonium acetate and 0.17 g of sodium cyanoborohydride in 12 ml of methanol was stirred at 60° C. for 17 hours. After the removal of the solvent under reduced pressure, the residue was taken up in 50 ml of ethyl acetate and washed twice with 30 ml of 0.5 N aqueous sodium hydroxide solution and 30 ml of saturated aqueous sodium chloride solution. The organic phase was dried over MgSO4 and concentrated by rotary evaporation. The crude product was subjected to a chiral separation.

후처리

  1. customAfter the removal of the solvent under reduced pressure
  2. washwashed twice with 30 ml of 0.5 N aqueous sodium hydroxide solution and 30 ml of saturated aqueous sodium chloride solution
  3. dry with materialThe organic phase was dried over MgSO4
  4. concentrationconcentrated by rotary evaporation
  5. customThe crude product was subjected to a chiral separation

출처 및 근거

ORD 기록
ord-862b77b448334435a0c2e674fe13fedc
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08828994B2

연결된 노트

불러오는 중…