Ethylene Glycol → 5-Methoxy-3-phenyl-1,2,3,4-tetrahydro-1-naphthalene carboxylic acid
반응식
C(C1[C:12]2[C:7](=[C:8]([O:13][CH3:14])[CH:9]=[CH:10][CH:11]=2)[CH2:6][CH:5]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH2:4]1)#N.[OH-:21].[K+].Cl.[CH2:24]([OH:27])[CH2:25]O>>[CH3:14][O:13][C:8]1[CH:9]=[CH:10][CH:11]=[C:12]2[C:7]=1[CH2:6][CH:5]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[CH2:4][CH:25]2[C:24]([OH:27])=[O:21]참가 물질
5
반응 조건
- 온도
- -20 °C
실험 절차
A mixture of 5.03 g (19.1 mmol) of 1-cyano-5-methoxy-3-phenyl-1,2,3,4-tetrahydronaphthalene, from Step 2, 40 mL of 5% aqueous potassium hydroxide solution and 90 mL of ethylene glycol is heated at reflux temperature for 8 h. The reaction mixture is then cooled to -20° C. and made acidic by the addition of cold concentrated aqueous hydrochloric acid solution. The acidic solution is extracted with methylene chloride and the organic extracts are washed with brine, dried over anhydrous magnesium sulfate, filtered and evaporated to give the title compound which is used in the next step without purification.
후처리
- temperatureat reflux temperature for 8 h
- extractionThe acidic solution is extracted with methylene chloride
- washthe organic extracts are washed with brine
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltered
- customevaporated
출처 및 근거
- ORD 기록
- ord-fc91d22e97bb4fbd813fd6436c68419a
- 출처 데이터셋
- uspto-grants-1991_02
- 특허 번호
- US04994486
반응 노트
불러오는 중…