Potassium Carbonate → Ciprofibrate

HRID 1605123

반응식

HRID 1605123 반응식
C(C1C=CC(OC(C)(C)C(O)=O)=CC=1)(=O)C.BrC(C)(C)C(OCC)=O.C(=O)([O-])[O-].[K+].[K+].[Cl:32][C:33]1([Cl:51])[CH2:35][CH:34]1[C:36]1[CH:50]=[CH:49][C:39]([O:40][C:41]([CH3:48])([CH3:47])[C:42]([O:44][CH2:45]C)=[O:43])=[CH:38][CH:37]=1.[OH-].[Na+]>C(#N)C>[Cl:32][C:33]1([Cl:51])[CH2:35][CH:34]1[C:36]1[CH:50]=[CH:49][C:39]([O:40][C:41]([CH3:48])([CH3:47])[C:42]([O:44][CH3:45])=[O:43])=[CH:38][CH:37]=1.[Cl:32][C:33]1([Cl:51])[CH2:35][CH:34]1[C:36]1[CH:50]=[CH:49][C:39]([O:40][C:41]([CH3:48])([CH3:47])[C:42]([OH:44])=[O:43])=[CH:38][CH:37]=1

참가 물질

8

반응물 5

HCID 11430Potassium CarbonateHCID 11745Propanoic acid, 2-bromo-2-methyl-, ethyl ester2회HCID 14798Sodium HydroxideHCID 103600Ethyl 2-[4-(2,2-dichlorocyclopropyl)phenoxy]-2-methylpropionateHCID 104106Propanoic acid, 2-(4-acetylphenoxy)-2-methyl-

생성물 2

HCID 2763CiprofibrateHCID 9944254Ciprofibrate Impurity D

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

Alternatively, methyl 2-[p-(2,2-dichlorocyclopropyl)phenoxy]-2-methylpropionate was prepared from 20 g. of p-(2,2-dichlorocyclopropyl)phenol [Example 24, part (a)], 38 g. of ethyl 2-bromo-2-methylpropionate and 42 g. of potassium carbonate in 100 ml. of acetonitrile. The ethyl 2-bromo-2-methylpropionate was added in two equal portions, the second portion being added after seven hours of heating at reflux. The reaction mixture was heated at reflux for about three days and the product isolated to give 32 g. of ethyl 2-[p-(2,2-dichlorocyclopropyl)phenoxy]-2-methylpropionate. The latter was hydrolyzed in the usual manner with ethanolic sodium hydroxide to produce 2-[p-(2,2-dichlorocyclopropyl)phenoxy]-2-methylpropionic acid, identical with the compound formed in Example 24, part (b).

후처리

  1. additionthe second portion being added after seven hours
  2. temperatureof heating
  3. temperatureat reflux
  4. temperatureThe reaction mixture was heated
  5. temperatureat reflux for about three days
  6. customthe product isolated
  7. customto give 32 g

출처 및 근거

ORD 기록
ord-2c9e5d49e228447185367f2eb6f4eab1
출처 데이터셋
uspto-grants-1976_04
특허 번호
US03948973

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