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Ethyl Salicylate → HCID 178449046, 화합물

HRID 130570
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HRID 130570 반응식
[C:1]([O:10]CC)(=[O:9])[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[OH:4].[OH-].[CH2:14]([N+:18]([CH2:27][CH2:28][CH2:29][CH3:30])([CH2:23][CH2:24][CH2:25][CH3:26])[CH2:19][CH2:20][CH2:21][CH3:22])[CH2:15][CH2:16][CH3:17]>O>[C:1]([O-:10])(=[O:9])[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[OH:4].[CH2:27]([N+:18]([CH2:14][CH2:15][CH2:16][CH3:17])([CH2:19][CH2:20][CH2:21][CH3:22])[CH2:23][CH2:24][CH2:25][CH3:26])[CH2:28][CH2:29][CH3:30]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 8365Ethyl SalicylateHCID 2723671Tetrabutylammonium Hydroxide

생성물 1

HCID 178449046HCID 178449046, 화합물

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
60 °C

실험 절차

A glass flask with reflux condenser, heatable oil bath, mechanical stirrer and internal thermometer was charged at room temperature with 35.90 g of ethyl salicylate and 282.13 g of water and these components were stirred together thoroughly. Subsequently 139.98 g of tetrabutylammonium hydroxide (40% strength in water) were added and the reaction mixture was heated to 60° C. It was stirred at 60° C. for one hour (the contents of the flask become clear). Then the reaction mixture was cooled and the water was distilled off under reduced pressure, 20 mbar, at 30-45° C. The residue was taken up at 60° C. in 200 ml of toluene. Subsequently the mixture was redistilled. The residue was recrystallized from 50 ml of butyl acetate. The product was filtered off, washed with butyl acetate and dried at 80° C. and 10 mbar in a vacuum drying cabinet. This gave a white solid having a melting point of 93° C.

후처리

  1. temperatureA glass flask with reflux condenser, heatable oil bath, mechanical stirrer
  2. stirringIt was stirred at 60° C. for one hour (the contents of the flask
  3. temperatureThen the reaction mixture was cooled
  4. distillationthe water was distilled off under reduced pressure, 20 mbar, at 30-45° C
  5. customwas taken up at 60° C. in 200 ml of toluene
  6. distillationSubsequently the mixture was redistilled
  7. customThe residue was recrystallized from 50 ml of butyl acetate
  8. filtrationThe product was filtered off
  9. washwashed with butyl acetate
  10. customdried at 80° C.
  11. custom10 mbar in a vacuum drying cabinet
  12. customThis gave a white solid

출처 및 근거

ORD 기록
ord-9b461631879345bd92daf1ca4edaa640
출처 데이터셋
uspto-grants-2008_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07381785B2

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