Potassium Carbonate → HCID 14720303、化合物

HRID 2351977ノート

反応式

HRID 2351977 の反応式
ClC.[CH3:3][C:4]1[CH:9]=[C:8]([CH3:10])[CH:7]=[CH:6][C:5]=1[NH:11][CH2:12][C:13]1[CH:14]=[N:15][CH:16]=[CH:17][CH:18]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:25]([S:29](Cl)(=[O:31])=[O:30])[CH2:26][CH2:27][CH3:28]>C(=O)(O)[O-].[Na+]>[CH3:3][C:4]1[CH:9]=[C:8]([CH3:10])[CH:7]=[CH:6][C:5]=1[N:11]([CH2:12][C:13]1[CH:14]=[N:15][CH:16]=[CH:17][CH:18]=1)[S:29]([CH2:25][CH2:26][CH2:27][CH3:28])(=[O:31])=[O:30]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 754301-Butanesulfonyl chlorideHCID 19844836HCID 19844836、化合物

生成物 1

HCID 14720303HCID 14720303、化合物

試薬・触媒・溶媒 1

HCID 516892Sodium Bicarbonate溶媒

実験手順

A 4.2 g. portion of 3-(2,4-dimethylphenylaminomethyl)pyridine chloromethane, and to it were added 4.1 g. of potassium carbonate and 4.7 g. of butanesulfonyl chloride. The mixture was stirred at ambient temperature for 4 days, and then was stirred under gentle reflux for several days more. It was then diluted with aqueous sodium bicarbonate and extracted with dichloromethane, and the organic layer was dried over magnesium sulfate and evaporated to an oil. The oil was applied to a silica gel column and eluted with dichloromethane and then with chloroform to obtain 0.75 g. of the desired product.

後処理

  1. stirringwas stirred
  2. temperatureunder gentle reflux for several days more
  3. extractionextracted with dichloromethane
  4. dry with materialthe organic layer was dried over magnesium sulfate
  5. customevaporated to an oil
  6. washeluted with dichloromethane
  7. customwith chloroform to obtain 0.75 g

出典と根拠

ORDレコード
ord-f1232f9bdfa44a5f9760ea108619adba
出典データセット
uspto-grants-1989_10
特許番号
US04874775

反応ノート

読み込み中…