Pyridine → HCID 67827556、化合物

HRID 729048

反応式

HRID 729048 の反応式
S(Cl)(Cl)=O.[C:5]([O-:14])(=[O:13])[C:6]1[C:7](=[CH:9][CH:10]=[CH:11][CH:12]=1)[OH:8].[Na+].N1C=CC=CC=1>ClCCl>[C:5]([OH:14])(=[O:13])[C:6]1[C:7](=[CH:9][CH:10]=[CH:11][CH:12]=1)[OH:8].[OH:13][CH2:5][C:6]1[C:7]([OH:8])=[CH:9][CH:10]=[CH:11][CH:12]=1

参加物

5

反応物 3

HCID 1049PyridineHCID 24386Thionyl ChlorideHCID 16760658Sodium Salicylate

生成物 1

HCID 67827556HCID 67827556、化合物収率 60%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

実験手順

Thionyl chloride (1 mol) in dichloromethane (400 ml) was added dropwise and with constant stirring to a dispersion of sodium salicylate (1 mol) in dichloromethane (800 ml). The mixture was stirred for a further hour, then left to cool to room temperature, care being taken to avoid absorption of atmospheric moisture. This solution was then added dropwise and with vigorous stirring to a solution of Product A mol) and pyridine (2 mol) in dichloromethane (1200 ml). After addition was completed, the mixture was heated to 40° C., held at this temperature for 10 minutes and then allowed to cool. The reaction mixture was then washed several times with water and dilute acid until no traces of pyridine remained. The organic phase was then dried over anhydrous sodium sulphate, filtered and stripped of solvent to obtain saligenin salicylate in 60% yield.

後処理

  1. waitleft
  2. customabsorption of atmospheric moisture
  3. additionThis solution was then added dropwise
  4. additionAfter addition
  5. temperaturethe mixture was heated to 40° C.
  6. temperatureto cool
  7. washThe reaction mixture was then washed several times with water
  8. additiondilute acid until no traces of pyridine
  9. dry with materialThe organic phase was then dried over anhydrous sodium sulphate
  10. filtrationfiltered

出典と根拠

ORDレコード
ord-74f4896ab63344a5a18d4e4157830de0
出典データセット
uspto-grants-1991_09
特許番号
US05051454

関連ノート

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