Potassium Carbonate → HCID 67280827、化合物

HRID 2378344ノート

反応式

HRID 2378344 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 67280827HCID 67280827、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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%)

後処理

  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)

出典と根拠

ORDレコード
ord-67d678da1bc149b1b2e1e9212bc80dd7
出典データセット
uspto-grants-2008_12
特許番号
US07470790B2

反応ノート

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