Methanamine, N-methoxy-, hydrochloride (1:1) → HCID 87442638, 화합물

HRID 384872노트

반응식

HRID 384872 반응식
[C:1]([O:5][C:6]([NH:8][CH:9]([C:13]1[CH:18]=[CH:17][C:16]([Cl:19])=[C:15]([F:20])[CH:14]=1)[C:10]([OH:12])=O)=[O:7])([CH3:4])([CH3:3])[CH3:2].C(N(C(C)C)C(C)C)C.Cl.[CH3:31][NH:32][O:33][CH3:34].[B-](F)(F)(F)F.CN(C(ON1N=NC2C1=CC=CC=2)=[N+](C)C)C>CN(C)C=O.O>[C:1]([O:5][C:6](=[O:7])[NH:8][CH:9]([C:13]1[CH:18]=[CH:17][C:16]([Cl:19])=[C:15]([F:20])[CH:14]=1)[C:10](=[O:12])[N:32]([O:33][CH3:34])[CH3:31])([CH3:2])([CH3:3])[CH3:4]

참가 물질

7

반응물 4

HCID 81138Methanamine, N-methoxy-, hydrochloride (1:1)HCID 81531DiisopropylethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 22309186[(tert-butoxycarbonyl)amino](4-chloro-3-fluorophenyl)acetic acid

생성물 1

HCID 87442638HCID 87442638, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

To a solution of 6.00 g (19.76 mmol) rac-tert-butoxycarbonylamino-(4-chloro-3-fluoro-phenyl)-acetic acid in 146 ml dimethylformamide were added 20.71 ml (118.6 mmol) N-ethyl-diisopropylamine, 2.07 g (20.75 mmol) N,O-dimethylhydroxylamine hydrochloride and 8.26 g (24.70 mmol) 0-(1H-benzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium tetrafluoroborate (TBTU) and the solution stirred at ambient temperature for 30 min. The reaction mixture was diluted with water and the resulting suspension stirred for 15 min. The precipitate was filtered and washed with water and dried: 5.18 g rac-[(4-chloro-3-fluoro-phenyl)-(methoxy-methyl-carbamoyl)-methyl]-carbamic acid tert-butyl ester as colorless solid: MS (ISP): 347.2 (M+H)+ and 247.1 ((M-Boc)+H)+ (100%).

후처리

  1. stirringthe resulting suspension stirred for 15 min
  2. filtrationThe precipitate was filtered
  3. washwashed with water
  4. customdried

출처 및 근거

ORD 기록
ord-514de68b8d7c497e9914612c13412078
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08367838B2

반응 노트

불러오는 중…