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Water → HCID 86737101, 화합물

HRID 2057956
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HRID 2057956 반응식
[CH2:1]([C:8]1[CH:15]=[C:12]([CH:13]=O)[C:11]([OH:16])=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH:24](C(OCC)=O)[C:25]([O:27][CH2:28][CH3:29])=[O:26].O>CC(=O)CC>[CH2:1]([C:8]1[CH:9]=[CH:10][C:11]2[O:16][C:24]([C:25]([O:27][CH2:28][CH3:29])=[O:26])=[CH:13][C:12]=2[CH:15]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 69637Diethyl bromomalonateHCID 45126705-Benzyl-2-hydroxy-benzaldehyde

생성물 1

HCID 86737101HCID 86737101, 화합물

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

6.9 g of 1A was dissolved in 130 ml of 2-butanone. The solution was heated to reflux and 8.1 g of potassium carbonate was added. Then 7.8 g of diethyl bromomalonate was added, drop-by-drop over a 10-minute period. The mixture was stirred at reflux for 58 hours, then was cooled and filtered. The filtrate was concentrated under reduced pressure to leave an oil, which was poured into water. The mixture was extracted with ether. The extract was washed with 5% sodium hydroxide solution, then with water, dried (MgSO4), and concentrated under reduced pressure. The residue was recrystallized from methanol and dried over P2O5 to give 1, mp: 78°-79° C.

후처리

  1. temperatureThe solution was heated
  2. temperatureto reflux
  3. temperatureat reflux for 58 hours
  4. temperaturewas cooled
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated under reduced pressure
  7. customto leave an oil, which
  8. extractionThe mixture was extracted with ether
  9. washThe extract was washed with 5% sodium hydroxide solution
  10. dry with materialwith water, dried (MgSO4)
  11. concentrationconcentrated under reduced pressure
  12. customThe residue was recrystallized from methanol
  13. dry with materialdried over P2O5
  14. customto give 1, mp: 78°-79° C.

출처 및 근거

ORD 기록
ord-4f6353ca7a484d2a823b8c5cefdbecad
출처 데이터셋
uspto-grants-1980_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04213999

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