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Potassium Carbonate → HCID 59255051, 화합물

HRID 1809360
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HRID 1809360 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:13]([NH:15][CH2:16][CH:17]2[CH2:22][CH2:21][N:20](C(OC(C)(C)C)=O)[CH2:19][CH2:18]2)=[O:14])[C:5](=[O:12])[N:6]([CH:9]([CH3:11])[CH3:10])[C:7]=1[CH3:8].C(=O)([O-])[O-].[K+].[K+]>CO.Cl>[Cl:1][C:2]1[CH:3]=[C:4]([C:13]([NH:15][CH2:16][CH:17]2[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]2)=[O:14])[C:5](=[O:12])[N:6]([CH:9]([CH3:10])[CH3:11])[C:7]=1[CH3:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 59255047HCID 59255047, 화합물

생성물 1

HCID 59255051HCID 59255051, 화합물수율 94%

시약·촉매·용매 1

HCID 21893726Hydrochloride methanol용매

실험 절차

A mixture of tert-butyl 4-({[(5-chloro-1-isopropyl-6-methyl-2-oxo-1,2-dihydropyridin-3-yl)carbonyl]amino}methyl)piperidine-1-carboxylate as prepared in 6(1) (4.77 g, 11.2 mmol) in 10% hydrochloric acid methanol solution (30 mL) was stirred at room temperature for 18 h. The mixture was concentrated in vacuo. The residue was dissolved in methanol (15 mL) and tetrahydrofuran (15 mL). To the resulting solution was added potassium carbonate (3.0 g, 21.7 mmol) at room temperature, and the mixture was stirred at room temperature for 18 h. Then, the mixture was filtered through a pad of Celite, washed with methanol/tetrahydrofuran (v/v=1/1, 200 mL). The filtrate was concentrated in vacuo. The residue was chromatographed on a column of silica gel eluting with dichloromethane/methanol/25% ammonium hydroxide (v/v/v=10/1/0.2) to give 3.43 g (94%) of the title compound as a white solid.

후처리

  1. concentrationThe mixture was concentrated in vacuo
  2. dissolutionThe residue was dissolved in methanol (15 mL)
  3. stirringthe mixture was stirred at room temperature for 18 h
  4. filtrationThen, the mixture was filtered through a pad of Celite
  5. washwashed with methanol/tetrahydrofuran (v/v=1/1, 200 mL)
  6. concentrationThe filtrate was concentrated in vacuo
  7. customThe residue was chromatographed on a column of silica gel eluting with dichloromethane/methanol/25% ammonium hydroxide (v/v/v=10/1/0.2)

출처 및 근거

ORD 기록
ord-0d1721e8ef244c8887900f3c6654bb84
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08362038B2

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