Trifluoroacetic acid → HCID 54560552, 화합물

HRID 849855노트

반응식

HRID 849855 반응식
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

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 53973617HCID 53973617, 화합물

생성물 1

HCID 54560552HCID 54560552, 화합물수율 94.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

((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.

후처리

  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

출처 및 근거

ORD 기록
ord-1a0e0b96d2834ff48c770373a7e6ccd3
출처 데이터셋
uspto-grants-2000_01
특허 번호
US06013658

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