홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Potassium Hydroxide → 4'-(1-Methyl-heptyloxy)-4-biphenylcarboxylic acid

HRID 1789312
노트
인쇄 미리보기

반응식

HRID 1789312 반응식
C(OC(C1C=CC(C2C=CC(O)=CC=2)=CC=1)=O)C.[OH-].[K+].CC(OS(C1C(C)=CC=CC=1)(=O)=O)CCCCCC.C([O:42][C:43]([C:45]1[CH:50]=[CH:49][C:48]([C:51]2[CH:56]=[CH:55][C:54]([O:57][CH:58]([CH3:65])[CH2:59][CH2:60][CH2:61][CH2:62][CH2:63][CH3:64])=[CH:53][CH:52]=2)=[CH:47][CH:46]=1)=[O:44])C.[OH-].[Na+]>C(O)C.O.C1(C)C=CC=CC=1>[CH3:65][CH:58]([O:57][C:54]1[CH:55]=[CH:56][C:51]([C:48]2[CH:47]=[CH:46][C:45]([C:43]([OH:44])=[O:42])=[CH:50][CH:49]=2)=[CH:52][CH:53]=1)[CH2:59][CH2:60][CH2:61][CH2:62][CH2:63][CH3:64]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 5

HCID 14797Potassium HydroxideHCID 14798Sodium HydroxideHCID 4049156Ethyl 4'-hydroxy-4-biphenylcarboxylateHCID 136436484'-(1-Methyl-heptyloxy)-4-biphenylcarboxylic acid ethyl esterHCID 19990276Toluenesulfonic acid 1-methyl-heptyl ester

생성물 1

HCID 136436504'-(1-Methyl-heptyloxy)-4-biphenylcarboxylic acid
수율 65.8%

시약·촉매·용매 3

HCID 702Ethanol용매2회HCID 962Water용매HCID 1140Toluene용매

실험 절차

On the other hand, 4-hydroxy-4'-biphenylcarboxylic acid ethyl ester (IV) (38.7 g, 0.160 mol) was dissolved in ethanol (200 ml), and KOH (9 g, 0.160 mol) was added to and dissolved in the solution, followed by adding optically active toluenesulfonic acid 1-methyl-heptyl ester (50 g, 0.176 mol) obtained above, keeping the mixture under reflux for 4 hours, then cooling, adding toluene (200 ml) and 6N--HCl (50 ml), washing the resulting toluene layer with 2N--NaOH aqueous solution and further with water till the washing water became neutral, and distilling off toluene to obtain as a residue, optically active 4'-(1-methyl-heptyloxy)-4-biphenylcarboxylic acid ethyl ester (V) (38.6 g). This product (38.6 g, 0.109 mol) was dissolved in ethanol (6 ml), NaOH (5.3 g, 0.130 mol) and water (26 ml), followed by heating the solution under reflux for 10 minutes to deposit crystals, cooling, adding 6N--HCl (20 ml) to filter off crystals and further recrystallizing from acetic acid to obtain optically active 4'-(1-methyl-heptyloxy)-4-biphenylcarboxylic acid (VI) (23.4 g). This product exhibited liquid crystal phases and the phase transition points were as follows: C-SC* point 160° C., SC*-Ch point 177° C. and Ch-I point 196° C.

후처리

  1. dissolutiondissolved in the solution
  2. customobtained above,
  3. temperatureunder reflux for 4 hours
  4. temperaturecooling
  5. washHCl (50 ml), washing the resulting toluene layer with 2N
  6. distillationdistilling off toluene
  7. customto obtain as a residue
  8. temperatureby heating the solution
  9. temperatureunder reflux for 10 minutes
  10. temperaturecooling
  11. additionadding 6N
  12. filtrationHCl (20 ml) to filter off crystals
  13. customfurther recrystallizing from acetic acid

출처 및 근거

ORD 기록
ord-1f7059ca42634837b7b995e414e4f63a
출처 데이터셋
uspto-grants-1987_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04689176

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트