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

Triethylamine → (R)-N-(2-(3-(3-methoxyphenyl)-3-phenyl-2-propen-1-yloxy)ethyl)-3-piperidinecarboxylic acid ethyl ester

HRID 566554
노트
인쇄 미리보기

반응식

HRID 566554 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:9]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)=[CH:10][CH2:11][O:12][CH2:13][CH2:14]O)[CH:6]=[CH:7][CH:8]=1.C(N(CC)CC)C.CS(Cl)(=O)=O.[NH:34]1[CH2:39][CH2:38][CH2:37][C@@H:36]([C:40]([O:42][CH2:43][CH3:44])=[O:41])[CH2:35]1.C(=O)([O-])[O-].[K+].[K+]>C1(C)C=CC=CC=1.O>[CH2:43]([O:42][C:40]([C@@H:36]1[CH2:37][CH2:38][CH2:39][N:34]([CH2:14][CH2:13][O:12][CH2:11][CH:10]=[C:9]([C:5]2[CH:6]=[CH:7][CH:8]=[C:3]([O:2][CH3:1])[CH:4]=2)[C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=2)[CH2:35]1)=[O:41])[CH3:44]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 8471TriethylamineHCID 11430Potassium CarbonateHCID 31297Methanesulfonyl chlorideHCID 185582ethyl (3R)-piperidine-3-carboxylateHCID 54300857HCID 54300857, 화합물

생성물 1

HCID 54305203(R)-N-(2-(3-(3-methoxyphenyl)-3-phenyl-2-propen-1-yloxy)ethyl)-3-piperidinecarboxylic acid ethyl ester
수율 61.1%

시약·촉매·용매 2

HCID 962Water용매HCID 1140Toluene용매2회

반응 조건

온도
5 °C

실험 절차

A mixture of 2-(3-(3-methoxyphenyl)-3-phenyl-2-propen-1-yloxy)ethanol (52 g, 0.18 mol) and triethylamine (46 g, 0.46 mol) in dry toluene (200 ml) kept under a nitrogen atmosphere was cooled below 10 C and a solution of methanesulphonyl chloride (41.7 g, 0.36 mol) in dry toluene (200 ml) was added dropwise keeping the temperature below 10° C. When addition was complete the reaction mixture was stirred for 1 h at 5° C. and then for 0.5 h at approximately 15° C. Water was added (250 ml) and the mixture was stirred at room temperature for 0.5 h. The separated organic phase was washed with a 5% sodium bicarbonate solution, brine and dried (Na2SO4). The mixture was filtered and the filtrate was reduced to approximately 500 ml in vacuo. Ethyl (R)-3-piperidinecarboxylate (57.2 g, 0.36 mol) and potassium carbonate (62.8 g, 0.46 mol) were added and the mixture was heated at reflux temperature for 48 h. The cooled reaction mixture was filtered and the solid was washed with toluene and ethyl acetate successively. The combined organic filtrates was evaporated in vacuo to an oily residue which was dissolved into ethyl acetate (250 ml). Water (150 ml) was added and pH was adjusted to 4 with 10% citric acid solution. The phases were separated and the organic phase was washed with water (150 ml). The combined aqueous phases was extracted with ethyl acetate (150 ml) and then discarded. The combined organic phases was washed with a 5% sodium bicarbonate solution, brine, dried (Na2SO4) and the solvent evaporated in vacuo. The residue was dissolved in toluene (150 ml) and a solution of tartaric acid (42 g) in water (120 ml) was added. The phases were separated and the organic phase was extracted with another solution of tartaric acid (12 g) in water (50 ml). The combined aqueous extracts was extracted with ethyl acetate (200 ml) which was discarded. Ethyl acetate (200 ml) was added to the acidic aqueous phase which was made alkaline with excess of a sodium bicarbonate solution. The separated organic phase was washed with brine and dried (Na2SO4). The solvent was evaporated in vacuo to give 46.6 g (60%) of (R)-N-(2-(3-(3-methoxyphenyl)-3-phenyl-2-propen1-yloxy)ethyl)-3-piperidinecarboxylic acid ethyl ester as an oil.

후처리

  1. temperaturewas cooled below 10 C
  2. customthe temperature below 10° C
  3. additionWhen addition
  4. waitfor 0.5 h at approximately 15° C
  5. stirringthe mixture was stirred at room temperature for 0.5 h
  6. washThe separated organic phase was washed with a 5% sodium bicarbonate solution, brine
  7. dry with materialdried (Na2SO4)
  8. filtrationThe mixture was filtered
  9. temperaturethe mixture was heated
  10. temperatureat reflux temperature for 48 h
  11. customThe cooled reaction mixture
  12. filtrationwas filtered
  13. washthe solid was washed with toluene and ethyl acetate successively
  14. customThe combined organic filtrates was evaporated in vacuo to an oily residue which
  15. dissolutionwas dissolved into ethyl acetate (250 ml)
  16. additionWater (150 ml) was added
  17. customThe phases were separated
  18. washthe organic phase was washed with water (150 ml)
  19. extractionThe combined aqueous phases was extracted with ethyl acetate (150 ml)
  20. washThe combined organic phases was washed with a 5% sodium bicarbonate solution, brine
  21. dry with materialdried (Na2SO4)
  22. customthe solvent evaporated in vacuo
  23. dissolutionThe residue was dissolved in toluene (150 ml)
  24. additiona solution of tartaric acid (42 g) in water (120 ml) was added
  25. customThe phases were separated
  26. extractionthe organic phase was extracted with another solution of tartaric acid (12 g) in water (50 ml)
  27. extractionThe combined aqueous extracts was extracted with ethyl acetate (200 ml) which
  28. additionEthyl acetate (200 ml) was added to the acidic aqueous phase which
  29. washThe separated organic phase was washed with brine
  30. dry with materialdried (Na2SO4)
  31. customThe solvent was evaporated in vacuo

출처 및 근거

ORD 기록
ord-27e7ce89ddc1458eaf4cd4f175959e68
출처 데이터셋
uspto-grants-2001_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06174898B1

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트