Potassium Carbonate → HCID 67280827, 화합물

HRID 1671617노트

반응식

HRID 1671617 반응식
[C:1]([O:5][C:6](=[O:21])[NH:7][C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([CH2:14][CH:15]2[CH:19]([OH:20])[CH2:18][NH:17][CH2:16]2)[N:9]=1)([CH3:4])([CH3:3])[CH3:2].[C:22]([O-:25])([O-])=[O:23].[K+].[K+]>CN(C=O)C>[C:1]([O:5][C:6](=[O:21])[NH:7][C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([CH2:14][CH:15]2[CH:19]([OH:20])[CH2:18][N:17]([CH2:13][CH2:8][NH:7][C:22]([O:25][C:1]([CH3:4])([CH3:3])[CH3:2])=[O:23])[CH2:16]2)[N:9]=1)([CH3:4])([CH3:2])[CH3:3]

참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 598580021,1-Dimethylethyl N-[6-[(4-hydroxy-3-pyrrolidinyl)methyl]-2-pyridinyl]carbamate

생성물 1

HCID 67280827HCID 67280827, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of [6-(4-hydroxy-pyrrolidin-3-ylmethyl)-pyridin-2-yl]-carbamic acid tert-butyl ester II-1 (0.01 mol), (2-bromo-ethyl)-carbamic acid tert-butyl (0.012 mol), anhydrous K2CO3 (0.02 mol) in 50 mL anhydrous DMF was stirred at room temperature overnight. Solids were filtered off. The filtrate was evaporated under reduced pressure. The residue was partitioned between EtOAc and water. The organic layer was washed with brine, dried over anhydrous Na2SO4, and evaporated in vacuo. The obtained residue was purified by column chromatography (silica gel, CH2Cl2:MeOH, 9:1). (57%)

후처리

  1. filtrationSolids were filtered off
  2. customThe filtrate was evaporated under reduced pressure
  3. customThe residue was partitioned between EtOAc and water
  4. washThe organic layer was washed with brine
  5. dry with materialdried over anhydrous Na2SO4
  6. customevaporated in vacuo
  7. customThe obtained residue was purified by column chromatography (silica gel, CH2Cl2:MeOH, 9:1)

출처 및 근거

ORD 기록
ord-c3aa29300dc34e698486f713ac01297f
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07994326B2

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