Potassium Hydroxide → 2'-Chloro-4-biphenylylglycolic acid

HRID 267382

반응식

HRID 267382 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[CH:13]=[CH:12][C:11]([CH:14]([OH:20])[C:15]([O:17]CC)=[O:16])=[CH:10][CH:9]=1.[OH-].[K+]>C(O)(C)C>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[CH:13]=[CH:12][C:11]([CH:14]([OH:20])[C:15]([OH:17])=[O:16])=[CH:10][CH:9]=1

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 21556089Ethyl 2'-chloro-4-biphenylylglycolate

생성물 1

HCID 215230142'-Chloro-4-biphenylylglycolic acid

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

To a solution of 0.144 moles of ethyl 2'-chloro-4-biphenylylglycolate dissolved in 220 ml. of isopropanol is added 38 g. (0.7 mole) of potassium hydroxide. This mixture is then heated at reflux temperature in a nitrogen atmosphere. The solution is concentrated in vacuo to a viscous oil, which is then dissolved in 500 ml. of water and filtered. The filtrate is acidified with 10% HCl and the precipitate is taken up in ether. The ether layer is dried, filtered and the filtrate concentrated to dryness. Recrystallization of residue from benzene-cyclohexane 1:1 gives 2'-chloro-4-biphenylylglycolic acid.

후처리

  1. temperatureThis mixture is then heated
  2. temperatureat reflux temperature in a nitrogen atmosphere
  3. concentrationThe solution is concentrated in vacuo to a viscous oil, which
  4. dissolutionis then dissolved in 500 ml
  5. filtrationof water and filtered
  6. dry with materialThe ether layer is dried
  7. filtrationfiltered
  8. concentrationthe filtrate concentrated to dryness
  9. customRecrystallization of residue from benzene-cyclohexane 1:1

출처 및 근거

ORD 기록
ord-10f30f8f91ca40458e6a5415b9b15da9
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03941821

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