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Potassium Carbonate → HCID 84002672, 화합물

HRID 509913
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HRID 509913 반응식
Cl.[C:2]([O:6][C:7](=[O:15])[NH:8][CH:9]1[CH2:14][CH2:13][CH2:12][NH:11][CH2:10]1)([CH3:5])([CH3:4])[CH3:3].I[CH2:17][C:18]([O:20][CH2:21][CH3:22])=[O:19].C([O-])([O-])=O.[K+].[K+]>C(#N)C>[CH2:21]([O:20][C:18](=[O:19])[CH2:17][N:11]1[CH2:12][CH2:13][CH2:14][CH:9]([NH:8][C:7]([O:6][C:2]([CH3:5])([CH3:3])[CH3:4])=[O:15])[CH2:10]1)[CH3:22]
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참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 12183Ethyl iodoacetateHCID 44891089Carbamic acid, N-3-piperidinyl-, 1,1-dimethylethyl ester, hydrochloride (1:1)

생성물 1

HCID 84002672HCID 84002672, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a solution of piperidin-3-yl-carbamic acid tert-butyl ester hydrochloride (1.0 g, 4.2 mmol) and ethyl iodoacetate (0.99 g, 4.6 mmol) in acetonitrile (30 mL) is added K2CO3 (1.5 g, 10.5 mmol) and the mixture stirred overnight at room temperature. Volatiles are evaporated under reduced pressure and the residue taken up with water and extracted twice with ethyl acetate. The organic phase is dried over MgSO4 and evaporated under reduced pressure. The resulting material is purified via chromatography over silica gel eluting with a mixture of EtOAc/MeOH (95:5 v/v). Yield: 0.8 g.

후처리

  1. customVolatiles are evaporated under reduced pressure
  2. extractionextracted twice with ethyl acetate
  3. dry with materialThe organic phase is dried over MgSO4
  4. customevaporated under reduced pressure
  5. customThe resulting material is purified via chromatography over silica gel eluting with a mixture of EtOAc/MeOH (95:5 v/v)

출처 및 근거

ORD 기록
ord-d42b9bcf75dd469d83693c66624f7a86
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09096548B2

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