Water → HCID 59625636, 화합물

HRID 2192811노트

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HRID 2192811 반응식
C([O:4][CH2:5][CH:6]1[CH2:11][CH:10]([N:12]([C:17]([C:19]2[C:20]([NH:29][CH2:30][C:31]3[O:32][CH:33]=[CH:34][CH:35]=3)=[N:21][C:22]([C:25]([CH3:28])([CH3:27])[CH3:26])=[N:23][CH:24]=2)=[O:18])[CH2:13][CH:14]([CH3:16])[CH3:15])[CH2:9][N:8]([C:36]([O:38][C:39]([CH3:42])([CH3:41])[CH3:40])=[O:37])[CH2:7]1)(=O)C.O.[OH-].[Na+]>CO>[C:25]([C:22]1[N:21]=[C:20]([NH:29][CH2:30][C:31]2[O:32][CH:33]=[CH:34][CH:35]=2)[C:19]([C:17]([N:12]([CH2:13][CH:14]([CH3:16])[CH3:15])[CH:10]2[CH2:11][CH:6]([CH2:5][OH:4])[CH2:7][N:8]([C:36]([O:38][C:39]([CH3:42])([CH3:41])[CH3:40])=[O:37])[CH2:9]2)=[O:18])=[CH:24][N:23]=1)([CH3:28])([CH3:27])[CH3:26]

참가 물질

5

반응물 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 59625506HCID 59625506, 화합물

생성물 1

HCID 59625636HCID 59625636, 화합물수율 97.9%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
70 °C

실험 절차

To a solution of tert-butyl 3-[(acetyloxy)methyl]-5-[({2-tert-butyl-4-[(furan-2-ylmethyl)amino]pyrimidin-5-yl}carbonyl)(2-methylpropyl)amino]piperidine-1-carboxylate (780 mg) in methanol (10 ml)-water (9 ml) was added 8 M aqueous sodium hydroxide solution (0.83 ml), and the mixture was stirred at 70° C. for 7 hr and extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was subjected to silica gel column chromatography, and the fraction eluted with ethyl acetate-hexane (5:95-100:0) was concentrated under reduced pressure to give the object compound (709 mg).

후처리

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. washthe fraction eluted with ethyl acetate-hexane (5:95-100:0)
  6. concentrationwas concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-9a1363dc62074ebe8efc00fc45839e6e
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08329691B2

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