Tetrahydrofuran → HCID 70050348, 화합물

HRID 1647090노트

반응식

HRID 1647090 반응식
[NH2:1][C:2]1[CH:11]=[CH:10][C:5](C(OC)=O)=[CH:4][CH:3]=1.Cl[C:13]([O:16][C:17](Cl)=[O:18])(Cl)Cl.[CH2:20]([O:27][C:28](=[O:34])[C@H:29]([CH:31]([CH3:33])[CH3:32])[NH2:30])[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.C(N(CC)CC)C.[O:42]1CCC[CH2:43]1>>[CH2:20]([O:27][C:28](=[O:34])[C@H:29]([CH:31]([CH2:32][C:17]([O:16][CH3:13])=[O:18])[CH3:33])[NH:30][C:43]([NH:1][C:2]1[CH:3]=[CH:4][CH:5]=[CH:10][CH:11]=1)=[O:42])[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1

참가 물질

6

반응물 5

HCID 8028TetrahydrofuranHCID 8471TriethylamineHCID 10426DiphosgeneHCID 12082Methyl 4-aminobenzoateHCID 6950584benzyl (2S)-2-amino-3-methylbutanoate

생성물 1

HCID 70050348HCID 70050348, 화합물

실험 절차

To a solution of methyl p-aminobenzoate (0.4 g) in tetrahydrofuran (10 ml) was added trichloromethylchloroformate (0.31 g) and the mixture was allowed to stand overnight at room temperature. L-Valine benzyl ester (0.54 g) was added to the solution and the pH of the mixture was neutralized with triethylamine. After being stirred for 30 minutes at room temperature, the mixture was concentrated under reduced pressure and the residue was extracted with ethyl acetate (10 ml). The extract was washed with 1N-hydrochloric acid (10 ml) and aqueous sodium bicarbonate (10 ml) and concentrated to dryness to give 4-(methoxycarbonyl)phenylaminocarbonyl-L-valine benzyl ester (1.17 g).

후처리

  1. concentrationthe mixture was concentrated under reduced pressure
  2. extractionthe residue was extracted with ethyl acetate (10 ml)
  3. washThe extract was washed with 1N-hydrochloric acid (10 ml) and aqueous sodium bicarbonate (10 ml)
  4. concentrationconcentrated to dryness

출처 및 근거

ORD 기록
ord-1760c07e0d5546cf8f11bd102b954cdf
출처 데이터셋
uspto-grants-1995_07
특허 번호
US05430025

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