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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Acetone → HCID 22494013, 화합물

HRID 1435144
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HRID 1435144 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([OH:11])[C:5](=[CH:9][CH:10]=1)[C:6]([OH:8])=[O:7].C(=O)([O-])[O-].[K+].[K+].S(OCC)(O[CH2:22][CH3:23])(=O)=O.[CH3:27][C:28](C)=O>O>[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([O:8][CH2:22][CH3:23])=[O:7])=[C:4]([O:11][CH2:27][CH3:28])[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 180AcetoneHCID 6163Diethyl SulfateHCID 11430Potassium CarbonateHCID 787824-Chlorosalicylic acid

생성물 1

HCID 22494013HCID 22494013, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 4-chlorosalicylic acid (10.0 g, 57.94 mmol) and potassium carbonate (80 g, 0.58 mol) and diethyl sulphate (18.76 g, 0.122 mol) in acetone (150 ml) is heated at reflux with stirring for 24 h. The suspension is cooled and diluted with water (200 ml). Extract with diethyl ether (2×) and wash the extracts with water (2×) and brine. The organic phase is dried over magnesium sulphate, filtered and evaporated to a brown oil. The oil is purified using the combiflash on a 120 g silica cartridge eluting with isohexane-ethyl acetate (0 to 25% over 30 min.) to give ethyl 4-chloro-2-ethoxybenzoate as a colourless oil.

후처리

  1. temperatureis heated
  2. temperatureat reflux
  3. temperatureThe suspension is cooled
  4. extractionExtract with diethyl ether (2×)
  5. washwash the extracts with water (2×) and brine
  6. dry with materialThe organic phase is dried over magnesium sulphate
  7. filtrationfiltered
  8. customevaporated to a brown oil
  9. customThe oil is purified
  10. washeluting with isohexane-ethyl acetate (0 to 25% over 30 min.)

출처 및 근거

ORD 기록
ord-f48fffba2b9d4d468759770fcfd69cdb
출처 데이터셋
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07615648B2

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