Potassium Carbonate → HCID 14720346、化合物

HRID 2352003ノート

反応式

HRID 2352003 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][C:3]=1[NH:9][CH2:10][C:11]1[CH:12]=[N:13][CH:14]=[CH:15][CH:16]=1.C(=O)([O-])[O-].[K+].[K+].[CH3:23][S:24](Cl)(=[O:26])=[O:25]>ClCCl>[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][C:3]=1[N:9]([CH2:10][C:11]1[CH:12]=[N:13][CH:14]=[CH:15][CH:16]=1)[S:24]([CH3:23])(=[O:26])=[O:25]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 31297Methanesulfonyl chlorideHCID 14720345N-(2,4-Dimethylphenyl)-3-pyridinemethanamine

生成物 1

HCID 14720346HCID 14720346、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A 4.2 g. portion of 3-(2,4-dimethylphenylaminomethyl)pyridine was dissolved in 20 ml. of dichloromethane and 4.1 g. of potassium carbonate and 2.5 ml. of methanesulfonyl chloride were added. The mixture was stirred over the week-end under reflux, and was then extracted with 20 ml. of aqueous sodium bicarbonate. The organic phase was dried and evaporated under vacuum. The residue was dissolved in diethyl ether and the solution was separated from insolubles and evaporated under vacuum. The oil was dissolved in chloroform and chromatographed over silica gel, eluting with chloroform:ethyl acetate to obtain 2.5 g. of the desired product, m.p. 62°-65°.

後処理

  1. temperatureunder reflux
  2. extractionwas then extracted with 20 ml
  3. customThe organic phase was dried
  4. customevaporated under vacuum
  5. dissolutionThe residue was dissolved in diethyl ether
  6. customthe solution was separated from insolubles
  7. customevaporated under vacuum
  8. dissolutionThe oil was dissolved in chloroform
  9. customchromatographed over silica gel
  10. washeluting with chloroform
  11. customethyl acetate to obtain 2.5 g

出典と根拠

ORDレコード
ord-c171eccab5be47df84d51ba3e43722bc
出典データセット
uspto-grants-1989_10
特許番号
US04874775

反応ノート

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