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

Acetic acid, 2-(triphenylphosphoranylidene)-, ethyl ester → (E)-5,5-bis(4-methoxyphenyl)-2,4-pentadienoic acid

HRID 1110507
노트
인쇄 미리보기

반응식

HRID 1110507 반응식
COC1C=CC(C(C2C=CC(OC)=CC=2)=CC=O)=CC=1.C(C=P(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)(OCC)=O.C([O:48][C:49](=[O:70])/[CH:50]=[CH:51]/[CH:52]=[C:53]([C:62]1[CH:67]=[CH:66][C:65]([O:68][CH3:69])=[CH:64][CH:63]=1)[C:54]1[CH:59]=[CH:58][C:57]([O:60][CH3:61])=[CH:56][CH:55]=1)C>C(Cl)(Cl)(Cl)Cl.CO.[OH-].[Na+]>[CH3:69][O:68][C:65]1[CH:64]=[CH:63][C:62]([C:53]([C:54]2[CH:55]=[CH:56][C:57]([O:60][CH3:61])=[CH:58][CH:59]=2)=[CH:52]/[CH:51]=[CH:50]/[C:49]([OH:70])=[O:48])=[CH:67][CH:66]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 70670Acetic acid, 2-(triphenylphosphoranylidene)-, ethyl esterHCID 141685443,3-bis(4-Methoxyphenyl)-2-propenalHCID 86742567(E)-5,5-bis(4-methoxyphenyl)-2,4-pentadienoic acid ethyl ester

생성물 1

HCID 14347253(E)-5,5-bis(4-methoxyphenyl)-2,4-pentadienoic acid

시약·촉매·용매 3

HCID 887Methanol용매
HCID 5943
Carbon Tetrachloride
용매
HCID 14798Sodium Hydroxide용매

실험 절차

A mixture of 3,3-bis(4-methoxyphenyl)-2-propenal (22.7 g) and (carbethoxymethylene)triphenylphosphorane (30 g) in carbon tetrachloride (200 mL) was stirred overnight at room temperature and then at reflux for 5 hours to complete the reaction. The crude product (28.4 g) obtained from the usual work up consisted mainly of (E)-5,5-bis(4-methoxyphenyl)-2,4-pentadienoic acid ethyl ester. The crude ester (28.4 g) in a mixture of methanol (200 mL) and 2N sodium hydroxide solution (100 mL) was heated at reflux for 30 minutes, then most of the methanol was distilled from the reaction. The base mixture was cooled, diluted with water (300 mL), extracted with dichloromethane (3×400 mL) and then was poured into a stirred mixture of concentrated hydrochloric acid (50 mL), water (200 mL) and ice (200 mL). The yellow precipitate was filtered off, washed with water and dried. The material was triturated with ether (3×100 ml) to provide 21.5 g of (E)-5,5-bis(4-methoxyphenyl)-2,4-pentadienoic acid, mp 187°-189° C. Crystallization from dichloromethane-hexane furnished the pure acid, mp 189.5°-190.5° C. Anal. Calculated for C19H18O4C: 73.53; H, 5.85 Found: C, 73.34; H, 5.92.

후처리

  1. temperatureat reflux for 5 hours
  2. customthe reaction
  3. customThe crude product (28.4 g) obtained from the usual work
  4. temperaturewas heated
  5. temperatureat reflux for 30 minutes
  6. distillationmost of the methanol was distilled from the reaction
  7. temperatureThe base mixture was cooled
  8. additiondiluted with water (300 mL)
  9. extractionextracted with dichloromethane (3×400 mL)
  10. additionwas poured into a stirred mixture of concentrated hydrochloric acid (50 mL), water (200 mL) and ice (200 mL)
  11. filtrationThe yellow precipitate was filtered off
  12. washwashed with water
  13. customdried
  14. customThe material was triturated with ether (3×100 ml)

출처 및 근거

ORD 기록
ord-03f7ce9cb33b4aedb3a8327d75936841
출처 데이터셋
uspto-grants-1990_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04975438

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트