Potassium Carbonate → HCID 59625260, 화합물

HRID 2192835노트

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HRID 2192835 반응식
[C:1]([C:5]1[N:10]=[C:9]([NH:11][CH2:12][C:13]2[O:14][CH:15]=[CH:16][CH:17]=2)[C:8]([C:18]([N:20]([CH2:36][CH:37]([CH3:39])[CH3:38])[CH:21]2[CH2:26][CH:25]([CH2:27][OH:28])[CH2:24][N:23](C(OC(C)(C)C)=O)[CH2:22]2)=[O:19])=[CH:7][N:6]=1)([CH3:4])([CH3:3])[CH3:2].C(=O)([O-])[O-].[K+].[K+]>FC(F)(F)C(O)=O>[C:1]([C:5]1[N:10]=[C:9]([NH:11][CH2:12][C:13]2[O:14][CH:15]=[CH:16][CH:17]=2)[C:8]([C:18]([N:20]([CH:21]2[CH2:26][CH:25]([CH2:27][OH:28])[CH2:24][NH:23][CH2:22]2)[CH2:36][CH:37]([CH3:39])[CH3:38])=[O:19])=[CH:7][N:6]=1)([CH3:3])([CH3:4])[CH3:2]

참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 59625636HCID 59625636, 화합물

생성물 1

HCID 59625260HCID 59625260, 화합물수율 59.8%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

tert-Butyl 3-[({2-tert-butyl-4-[(furan-2-ylmethyl)amino]pyrimidin-5-yl}carbonyl)(2-methylpropyl)amino]-5-(hydroxymethyl)piperidine-1-carboxylate (50.0 mg) was dissolved in trifluoroacetic acid (50% 1,2-dichloroethane solution, 4 ml), and the mixture was stirred at room temperature for 1 hr. The reaction mixture was basified with saturated aqueous potassium carbonate solution, and the mixture was 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-methanol (50:50:0-100:0:0-85:0:15) was concentrated under reduced pressure to give the object compound (24.4 mg).

후처리

  1. extractionthe mixture was extracted 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-methanol (50:50:0-100:0:0-85:0:15)
  6. concentrationwas concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-886c5c89bdfa449a8c4e480576b38e88
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08329691B2

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