Sulfuric Acid → 701915-91-5

HRID 916534노트

반응식

HRID 916534 반응식
ClC1C=C(C(COC)[C:10](OC)=[O:11])C=C(Cl)C=1.S(=O)(=O)(O)O.[Cl:22][C:23]1[CH:24]=[C:25]([CH:32]=[C:33]([Cl:35])[CH:34]=1)[O:26][C:27](=[CH2:31])[C:28]([OH:30])=[O:29]>[OH-].[Na+].O>[Cl:22][C:23]1[CH:24]=[C:25]([CH:32]=[C:33]([Cl:35])[CH:34]=1)[O:26][CH:27]([CH2:31][O:11][CH3:10])[C:28]([OH:30])=[O:29]

참가 물질

6

반응물 3

HCID 1118Sulfuric AcidHCID 69114661HCID 69114661, 화합물HCID 69115163Methyl 2-(3,5-dichlorophenyl)-3-methoxypropionate

생성물 1

HCID 69114724701915-91-5

시약·촉매·용매 2

HCID 962Water용매2회HCID 14798Sodium Hydroxide용매

실험 절차

An emulsion of methyl 2-(3,5-dichlorophenyl)-3-methoxypropionate in sodium hydroxide (0.14 g) and water (2 ml) was stirred at ambient temperature for 2 hours when a clear solution was produced. The mixture was acidified with concentrated sulphuric acid (0.34 g), diluted with water then extracted with diethyl ether. The organic phase was separated, extracted with aqueous sodium hydrogen carbonate and the organic phase discarded. The basic aqueous extract was acidified with concentrated hydrochloric acid and extracted with diethyl ether. The extract was dried over magnesium sulphate and evaporated under reduced pressure to give a colourless oil, 0.50 g, containing a mixture of the required product and 2-(3,5-dichlorophenoxy)-acrylic acid in the ratio 2:1, which was used in the next Stage without further purification. 2-(3,5-Dichlorophenoxy)-3-methoxypropionic acid was characterised from its NMR spectrum.

후처리

  1. customwas produced
  2. extractionthen extracted with diethyl ether
  3. customThe organic phase was separated
  4. extractionextracted with aqueous sodium hydrogen carbonate
  5. extractionThe basic aqueous extract
  6. extractionextracted with diethyl ether
  7. dry with materialThe extract was dried over magnesium sulphate
  8. customevaporated under reduced pressure
  9. customto give a colourless oil, 0.50 g
  10. additioncontaining

출처 및 근거

ORD 기록
ord-0dedf610003341288aff6db99741f164
출처 데이터셋
uspto-grants-2007_09
특허 번호
US07271130B2

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