Water → HCID 57545186, 화합물

HRID 1661518노트

반응식

HRID 1661518 반응식
C[O:2][C:3](=[O:25])[CH:4]([C:18]1[CH:23]=[CH:22][C:21]([Br:24])=[CH:20][CH:19]=1)[O:5][C:6]1[CH:11]=[C:10]([O:12][CH2:13][CH3:14])[CH:9]=[C:8]([O:15][CH2:16][CH3:17])[CH:7]=1.O.C(=O)([O-])[O-].[K+].[K+]>CO>[Br:24][C:21]1[CH:20]=[CH:19][C:18]([CH:4]([O:5][C:6]2[CH:7]=[C:8]([O:15][CH2:16][CH3:17])[CH:9]=[C:10]([O:12][CH2:13][CH3:14])[CH:11]=2)[C:3]([OH:25])=[O:2])=[CH:23][CH:22]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 11430Potassium CarbonateHCID 57545204HCID 57545204, 화합물

생성물 1

HCID 57545186HCID 57545186, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

16.9 g (41.3 mmol) of methyl(4-bromophenyl)-(3,5-diethoxyphenoxy)acetate are dissolved in 80 ml of methanol and 8 ml of water under argon at RT, and 7.99 g (57.8 mmol) of potassium carbonate are added. The mixture is heated under RF for 4 h. After cooling, the precipitate is filtered off, the filtrate is concentrated, the residue is taken up in water and the solution is extracted four times with diethyl ether. The aqueous phase is adjusted to a pH of 2 by adding 10% strength hydrochloric acid and is extracted three times with ethyl acetate, and the combined ethyl acetate phases are washed with saturated sodium chloride solution, dried over sodium sulfate, filtered and concentrated. 16.1 g (99% of theory) of the product are obtained.

후처리

  1. temperatureThe mixture is heated under RF for 4 h
  2. temperatureAfter cooling
  3. filtrationthe precipitate is filtered off
  4. concentrationthe filtrate is concentrated
  5. extractionthe solution is extracted four times with diethyl ether
  6. additionby adding 10% strength hydrochloric acid
  7. extractionis extracted three times with ethyl acetate
  8. washthe combined ethyl acetate phases are washed with saturated sodium chloride solution
  9. dry with materialdried over sodium sulfate
  10. filtrationfiltered
  11. concentrationconcentrated
  12. custom16.1 g (99% of theory) of the product are obtained

출처 및 근거

ORD 기록
ord-19482c96379b47138c2ad592573849b3
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08030347B2

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