Hydrochloric Acid → HCID 178448469, 화합물

HRID 709212

반응식

HRID 709212 반응식
Cl.[CH3:2][C@@:3]([S:44]([CH3:47])(=[O:46])=[O:45])([CH2:14][CH2:15][N:16]1[CH:21]=[CH:20][C:19]([C:22]2[CH:27]=[CH:26][C:25]([O:28][CH2:29][C@H:30]3[CH2:35][CH2:34][C@@H:33]([O:36]C4CCCCO4)[CH2:32][CH2:31]3)=[CH:24][CH:23]=2)=[CH:18][C:17]1=[O:43])[C:4]([NH:6][O:7]C1CCCCO1)=[O:5]>O1CCOCC1>[OH:7][NH:6][C:4](=[O:5])[C@:3]([CH3:2])([S:44]([CH3:47])(=[O:46])=[O:45])[CH2:14][CH2:15][N:16]1[CH:21]=[CH:20][C:19]([C:22]2[CH:27]=[CH:26][C:25]([O:28][CH2:29][C@H:30]3[CH2:31][CH2:32][C@@H:33]([OH:36])[CH2:34][CH2:35]3)=[CH:24][CH:23]=2)=[CH:18][C:17]1=[O:43]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 178448466HCID 178448466, 화합물

생성물 1

HCID 178448469HCID 178448469, 화합물수율 90%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

HCl (1.0 N in water, 1.02 mL) was added to a solution of (2R)-2-methyl-2-(methylsulfonyl)-4-[2-oxo-4-(4-{[cis-4-(tetrahydro-2H-pyran-2-yloxy)cyclohexyl]methoxy}phenyl)pyridin-1 (2H)-yl]-N-(tetrahydro-2H-pyran-2-yloxy)butanamide (135 mg, 0.204 mmol) in 1,4-dioxane (5.0 mL). After 1 hour the reaction was concentrated to give a white solid. The solid was triturated with ethanol at 50° C., for 30 minutes. After cooling, filtration afforded the title compound as a white solid (90 mg, 90%). LCMS m/z 493.7 (M+1). 1H NMR (400 MHz, DMSO-d6) δ ppm 1.38-1.70 (m, 12H) 1.79 (br. s., 1H) 2.09-2.24 (m, 1H) 2.42 (ddd, J=13.07, 11.12, 4.68 Hz, 1H) 3.12 (s, 3H) 3.68-3.83 (m, 2H) 3.87 (d, J=6.63 Hz, 2H) 4.10 (d, J=6.44 Hz, 1H) 6.55-6.75 (m, 2H) 6.94-7.10 (m, 2H) 7.61-7.80 (m, 3H) 11.15 (br. s., 1H)

후처리

  1. concentrationAfter 1 hour the reaction was concentrated
  2. customto give a white solid
  3. customThe solid was triturated with ethanol at 50° C., for 30 minutes
  4. temperatureAfter cooling
  5. filtrationfiltration

출처 및 근거

ORD 기록
ord-caab5b3ccaa44b3d89189c48ab76f0a0
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09180123B2

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