Pyridine → HCID 67827556, 화합물

HRID 729048

반응식

HRID 729048 반응식
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

참가 물질

5

반응물 3

HCID 1049PyridineHCID 24386Thionyl ChlorideHCID 16760658Sodium Salicylate

생성물 1

HCID 67827556HCID 67827556, 화합물수율 60%

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-74f4896ab63344a5a18d4e4157830de0
출처 데이터셋
uspto-grants-1991_09
특허 번호
US05051454

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