Trifluoroacetic acid → HCID 18672430、化合物

HRID 1058245ノート

反応式

HRID 1058245 の反応式
C(O)(C(F)(F)F)=O.[Cl:8][C:9]1[CH:10]=[CH:11][C:12]([CH2:24][CH:25]([NH:29][C:30]2[CH:35]=[CH:34][C:33]([O:36][CH3:37])=[CH:32][CH:31]=2)[CH:26]([F:28])[F:27])=[C:13]([CH:23]=1)[CH2:14][NH:15]C(=O)OC(C)(C)C>C(Cl)Cl>[NH2:15][CH2:14][C:13]1[CH:23]=[C:9]([Cl:8])[CH:10]=[CH:11][C:12]=1[CH2:24][CH:25]([NH:29][C:30]1[CH:35]=[CH:34][C:33]([O:36][CH3:37])=[CH:32][CH:31]=1)[CH:26]([F:28])[F:27]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 18672390Tert-butyl 5-chloro-2-{3,3-difluoro-2-[(4-methoxyphenyl)amino]propyl}benzylcarbamate

生成物 1

HCID 18672430HCID 18672430、化合物収率 137.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

TFA (5.2 mL) was added to a stirred solution of tert-butyl 5-chloro-2-{3,3-difluoro-2-[(4-methoxyphenyl)amino]propyl}benzylcarbamate (0.516 g, 1.17 mmol) in CH2Cl2 (5.2 mL). After 1 h the solvent was evaporated in vacuo and the residue was partitioned between EtOAc and saturated aqueous Na2CO3. The EtOAc layer was dried (Na2SO4) and evaporated in vacuo to give N-{1-[2-(aminomethyl)-4-chlorobenzyl]-2,2-difluoroethyl}-N-(4-methoxyphenyl)amine (0.550 g) as a foam; MS m/z=341.1.

後処理

  1. customAfter 1 h the solvent was evaporated in vacuo
  2. customthe residue was partitioned between EtOAc and saturated aqueous Na2CO3
  3. dry with materialThe EtOAc layer was dried (Na2SO4)
  4. customevaporated in vacuo

出典と根拠

ORDレコード
ord-559c9629af0944898513ffd5bd931211
出典データセット
uspto-grants-2003_02
特許番号
US06515011B2

反応ノート

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