Hydrochloric Acid → 4-(5-Chloro-2-methoxyphenyl)butanoic acid

HRID 2074012노트

반응식

HRID 2074012 반응식
O=[C:2]([C:8]1[CH:13]=[C:12]([Cl:14])[CH:11]=[CH:10][C:9]=1[O:15][CH3:16])[CH2:3][CH2:4][C:5]([OH:7])=[O:6].C1(C)C=CC=CC=1.Cl>O.[Zn]>[C:5]([CH2:4][CH2:3][CH2:2][C:8]1[CH:13]=[C:12]([Cl:14])[CH:11]=[CH:10][C:9]=1[O:15][CH3:16])([OH:7])=[O:6]

참가 물질

6

반응물 3

HCID 313Hydrochloric Acid2회HCID 1140TolueneHCID 64970694-(5-Chloro-2-methoxy-phenyl)-4-oxo-butyric acid

생성물 1

HCID 124102564-(5-Chloro-2-methoxyphenyl)butanoic acid

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 962Water용매2회

반응 조건

온도
80 °C

실험 절차

The acid compound of step 1 above is added to a stirring mixture of toluene (22 ml), conc HCl (41 ml), water (17 ml) and the recovered product of mossy zinc (22.2 g) and mercuric chloride (2.2 g) stirred in an aqueous HCl solution for about 10 minutes. The mixture is stirred under reflux for about 16 hours, diluted with water, extracted with ethyl acetate and the organic layer is dried filtered and evaporated. The residue is taken up in 10% aqueous NaOH, and dimethyl sulfate (about 25 ml) added to the mixture which is heated to 80° C. The mixture is stirred at a constant temperature for about 4 hours, cooled, acidified and the resulting precipitate is filtered dried and used in the next step.

후처리

  1. temperatureunder reflux for about 16 hours
  2. extractionextracted with ethyl acetate
  3. customthe organic layer is dried
  4. filtrationfiltered
  5. customevaporated
  6. additiondimethyl sulfate (about 25 ml) added to the mixture which
  7. stirringThe mixture is stirred at a constant temperature for about 4 hours
  8. temperaturecooled
  9. filtrationthe resulting precipitate is filtered
  10. customdried

출처 및 근거

ORD 기록
ord-bf3bf98523004f5ab8749e5ca4dad799
출처 데이터셋
uspto-grants-1990_04
특허 번호
US04920219

반응 노트

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