Potassium Carbonate → HCID 59625260、化合物

HRID 2192835ノート

反応式

HRID 2192835 の反応式
[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]

参加物

4

反応物 2

HCID 11430Potassium CarbonateHCID 59625636HCID 59625636、化合物

生成物 1

HCID 59625260HCID 59625260、化合物収率 59.8%

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-886c5c89bdfa449a8c4e480576b38e88
出典データセット
uspto-grants-2012_12
特許番号
US08329691B2

反応ノート

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