HCID 54210448, 화합물 → HCID 53842374, 화합물

HRID 1789921노트

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HRID 1789921 반응식
[CH2:1]([O:3][C:4](=[O:26])[CH:5]([CH2:11][C:12]1[CH:13]=[N:14][C:15]([NH:18][C:19]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20])=[CH:16][CH:17]=1)[CH2:6][S:7]C(=O)C)[CH3:2]>C(O)C.N>[CH2:1]([O:3][C:4](=[O:26])[CH:5]([CH2:11][C:12]1[CH:13]=[N:14][C:15]([NH:18][C:19]([O:21][C:22]([CH3:23])([CH3:24])[CH3:25])=[O:20])=[CH:16][CH:17]=1)[CH2:6][S:7][S:7][CH2:6][CH:5]([C:4]([O:3][CH2:1][CH3:2])=[O:26])[CH2:11][C:12]1[CH:13]=[N:14][C:15]([NH:18][C:19]([O:21][C:22]([CH3:23])([CH3:24])[CH3:25])=[O:20])=[CH:16][CH:17]=1)[CH3:2]

참가 물질

4

반응물 1

HCID 54210448HCID 54210448, 화합물

생성물 1

HCID 53842374HCID 53842374, 화합물수율 98%

시약·촉매·용매 2

HCID 222Ammonia용매HCID 702Ethanol용매

실험 절차

3-Acetylsulfanyl-2-(6-tert-butoxycarbonylamino-pyridin-3-ylmethyl)-propionic acid ethyl ester (150 mg, 0.392 mmol) was dissolved in ethanol (15 mL) saturated with NH3 (g). After stirring for 160 min., the mixture was concentrated under reduced pressure. The residue was dissolved in EtOH (10 mL) whereafter a solution of 12 in EtOH (0.5 M, 0.784 mL) was added. The reaction was stirred for 30 min. at room temperature, then diluted with CH2Cl2, washed with saturated aqueous Na2S2O5 and saturated aqueous NaHCO3, dried, filtered and concentrated under reduced pressure to give 3-[3-(6-tert-butoxycarbonylamino-pyridin-3-yl)-2-ethoxycarbonyl-propyldisulfanyl]-2-(6-tert-butoxycarbonylamino-pyridin-3-ylmethyl)-propionic acid ethyl ester (130 mg, 98%).

후처리

  1. concentrationthe mixture was concentrated under reduced pressure
  2. dissolutionThe residue was dissolved in EtOH (10 mL) whereafter a solution of 12 in EtOH (0.5 M, 0.784 mL)
  3. additionwas added
  4. stirringThe reaction was stirred for 30 min. at room temperature
  5. additiondiluted with CH2Cl2
  6. washwashed with saturated aqueous Na2S2O5 and saturated aqueous NaHCO3
  7. customdried
  8. filtrationfiltered
  9. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-d892903084fa44d4a6cbbfbe8d170525
출처 데이터셋
uspto-grants-2006_07
특허 번호
US07071175B1

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