Trifluoroacetic acid → 4-[[(2-chloro-5-cyanophenyl)carbonyl]amino]-L-phenylalanine methyl ester

HRID 1976974ノート

反応式

HRID 1976974 の反応式
[CH3:1][O:2][C:3](=[O:32])[C@H:4]([CH2:13][C:14]1[CH:19]=[CH:18][C:17]([NH:20][C:21]([C:23]2[CH:28]=[C:27]([C:29]#[N:30])[CH:26]=[CH:25][C:24]=2[Cl:31])=[O:22])=[CH:16][CH:15]=1)[NH:5]C(OC(C)(C)C)=O.FC(F)(F)C(O)=O>ClCCl>[CH3:1][O:2][C:3](=[O:32])[C@H:4]([CH2:13][C:14]1[CH:15]=[CH:16][C:17]([NH:20][C:21]([C:23]2[CH:28]=[C:27]([C:29]#[N:30])[CH:26]=[CH:25][C:24]=2[Cl:31])=[O:22])=[CH:18][CH:19]=1)[NH2:5]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 539100724-[(2-chloro-5-cyanophenylcarbonyl)amino]-N-[(1,1-dimethylethoxy)carbonyl]-L-phenylalanine methyl ester

生成物 1

HCID 541933924-[[(2-chloro-5-cyanophenyl)carbonyl]amino]-L-phenylalanine methyl ester収率 100.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 4-[(2-chloro-5-cyanophenylcarbonyl)amino]-N-[(1,1-dimethylethoxy)carbonyl]-L-phenylalanine methyl ester (1.2 mmol, 0.55 g) in dichloromethane (12 mL) was added trifluoroacetic acid (3 mL) at room temperature. The reaction mixture was stirred for 15 hr at room temperature at which time TLC analysis of the mixture indicated the absence of starting material. The solvent was removed under vacuum and the residue was azeotrophed with toluene (2×10 mL) and dried under high vacuum to afford 0.43 g (100%) of an yellow solid. HR MS: Obs. mass, 358.0963. Calcd. mass, 358.0959 (M+H).

後処理

  1. customThe solvent was removed under vacuum
  2. customdried under high vacuum

出典と根拠

ORDレコード
ord-f0d41b6589934394b4a2b6e72965d30c
出典データセット
uspto-grants-2001_05
特許番号
US06229011B1

反応ノート

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