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Potassium Hydroxide → HCID 21180559, 화합물

HRID 1600861
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HRID 1600861 반응식
[OH-].[K+].C([O:5][C:6](=[O:32])[C:7]1[C:12]([O:13][C:14]2[CH:19]=[CH:18][C:17]3[O:20][CH2:21][O:22][C:16]=3[CH:15]=2)=[CH:11][CH:10]=[CH:9][C:8]=1[O:23][C:24]1[CH:29]=[CH:28][CH:27]=[C:26]([O:30][CH3:31])[CH:25]=1)C>CO>[CH2:21]1[O:20][C:17]2[CH:18]=[CH:19][C:14]([O:13][C:12]3[CH:11]=[CH:10][CH:9]=[C:8]([O:23][C:24]4[CH:29]=[CH:28][CH:27]=[C:26]([O:30][CH3:31])[CH:25]=4)[C:7]=3[C:6]([OH:32])=[O:5])=[CH:15][C:16]=2[O:22]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 21180554HCID 21180554, 화합물

생성물 1

HCID 21180559HCID 21180559, 화합물수율 67.3%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

KOH (371 mg, 5.7 mmol) that was dissolved in methanol was added to a solution of ethyl-2-(3-methoxyphenoxy)-6-[3,4-(methylenedioxy)phenoxy]benzoate (200 mg, 0.57 mmol) in methanol (5 ml). The mixture was heated under reflux for approximately 20 hours at which time TLL had indicated the formation of a polar material. The solvent was evaporated and the remaining residue was diluted with water (7 ml, pH≈7.5) and extracted with EtOAc (2×10 ml). The aqueous fraction was then acidified to pH~2.5 using concentrated HCl and then extracted with ethyl acetate (2×10 ml). Evaporation of solvents gave an off-white solid which was recrystallized from methanol/H2O to give 146 mg (67%) of a white solid, mp 146-148° C.

후처리

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for approximately 20 hours at which time TLL
  3. customThe solvent was evaporated
  4. additionthe remaining residue was diluted with water (7 ml, pH≈7.5)
  5. extractionextracted with EtOAc (2×10 ml)
  6. extractionextracted with ethyl acetate (2×10 ml)
  7. customEvaporation of solvents
  8. customgave an off-white solid which
  9. customwas recrystallized from methanol/H2O

출처 및 근거

ORD 기록
ord-c0764e30f00d46b893dc9d0a94242975
출처 데이터셋
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05977117

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