Methanamine, N-methoxy-, hydrochloride (1:1) → HCID 87442638、化合物

HRID 384872ノート

反応式

HRID 384872 の反応式
[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]

参加物

7

反応物 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

生成物 1

HCID 87442638HCID 87442638、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

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%).

後処理

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

出典と根拠

ORDレコード
ord-514de68b8d7c497e9914612c13412078
出典データセット
uspto-grants-2013_02
特許番号
US08367838B2

反応ノート

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