Trifluoroacetic acid → HCID 54560552、化合物

HRID 849855ノート

反応式

HRID 849855 の反応式
C(O[C:6](=O)[N:7]([C@@H:9]([C:21](=[O:40])[N:22]([C@@H:24]([C:32]1[O:33][C:34]([C:37](=[O:39])[NH2:38])=[N:35][N:36]=1)[CH2:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)[CH3:23])[CH2:10][C:11]1[CH:20]=[CH:19][C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH:12]=1)C)(C)(C)C.FC(F)(F)C(O)=O>ClCCl>[CH3:23][N:22]([C:21](=[O:40])[C@H:9]([NH:7][CH3:6])[CH2:10][C:11]1[CH:20]=[CH:19][C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH:12]=1)[C@@H:24]([C:32]1[O:33][C:34]([C:37]([NH2:38])=[O:39])=[N:35][N:36]=1)[CH2:25][C:26]1[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 53973617HCID 53973617、化合物

生成物 1

HCID 54560552HCID 54560552、化合物収率 94.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

((1R)-1-(((1R)-1-(5-Carbamoyl-[1,3,4]oxadiazol-2-yl)-2-phenylethyl)methylcarbamoyl)-2-(2-naphthyl)ethyl)methylcarbamic acid tert-butylester (300 mg, 0.55 mmol) was dissolved in dichloromethane (3 ml) and cooled to 0° C. Trifluoroacetic acid (3 ml) was added dropwise. The solution was stirred for 5 min at 0° C. The solvent was removed in vacuo. The residue was dissolved in ethyl acetate (5 ml), and the solvent was removed in vacuo. The residue was dissolved in ethyl acetate (5 ml), and the solvent was removed in vacuo. The residue was dissolved in 3M hydrogen chloride in ethyl acetate (5 ml), and the solvent was removed in vacuo. The residue was dissolved in 3M hydrogen chloride in ethyl acetate (5 ml), and the solvent was removed in vacuo to give 238 mg of crude 5-((1R)-1-(methyl((2R)-2-methylamino-3-(2-naphthyl)propionyl)amino)-2-phenylethyl)-[1,3,4]oxadiazol-2-carboxylic acid amide, which was used for the further synthesis.

後処理

  1. customThe solvent was removed in vacuo
  2. dissolutionThe residue was dissolved in ethyl acetate (5 ml)
  3. customthe solvent was removed in vacuo
  4. dissolutionThe residue was dissolved in ethyl acetate (5 ml)
  5. customthe solvent was removed in vacuo
  6. dissolutionThe residue was dissolved in 3M hydrogen chloride in ethyl acetate (5 ml)
  7. customthe solvent was removed in vacuo
  8. dissolutionThe residue was dissolved in 3M hydrogen chloride in ethyl acetate (5 ml)
  9. customthe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-1a0e0b96d2834ff48c770373a7e6ccd3
出典データセット
uspto-grants-2000_01
特許番号
US06013658

反応ノート

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