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

Phenylacetaldehyde → N-(1-Phenethyl-piperidin-3-ylmethyl)-N-phenyl-propionamide

HRID 1839181
노트
인쇄 미리보기

반응식

HRID 1839181 반응식
FC(F)(F)C(O)=O.[C:8]([N:15]1[CH2:20][CH2:19][CH2:18][CH:17]([CH2:21][N:22]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[C:23](=[O:26])[CH2:24][CH3:25])[CH2:16]1)(OC(C)(C)C)=O.[C:33]1([CH2:39]C=O)[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1.[BH-](OC(C)=O)(OC(C)=O)OC(C)=O.[Na+]>C(Cl)Cl>[CH2:8]([N:15]1[CH2:20][CH2:19][CH2:18][CH:17]([CH2:21][N:22]([C:27]2[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=2)[C:23](=[O:26])[CH2:24][CH3:25])[CH2:16]1)[CH2:39][C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 998PhenylacetaldehydeHCID 6422Trifluoroacetic acidHCID 5049666Sodium triacetoxyborohydrideHCID 12991578N-(1-Boc-piperidin-3-ylmethyl)-N-phenyl-propionamide

생성물 1

HCID 9950309N-(1-Phenethyl-piperidin-3-ylmethyl)-N-phenyl-propionamide

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

실험 절차

Trifluoroacetic acid (5 mL) was added dropwise to a solution of N-(1-Boc-piperidin-3-ylmethyl)-N-phenyl-propionamide 5 (1.21 g, 3.49 mmol) in 5 mL of dry CH2Cl2 at 0° C. (ice-water). The reaction mixture was stirred at room temperature for 30 minutes. TLC showed the reaction was complete. After removal of the solvents, the residue was dried under vacuum for 3 hrs. The crude compound was dissolved in DMF (5.0 mL) and phenylacetaldehyde (5.3 mL, 2M/in DMF, 5.3 mmol) was added. The mixture was stirred at room temperature for 30 min. NaB(OAc)3H (95%, 1.18 g, 5.3 mmol.) was introduced in one portion, and the mixture was stirred at room temperature overnight. The mixture was quenched with 10 mL of aqueous potassium carbonate (sat.), then extracted with ethyl acetate (3×60 mL). The extracts were combined and washed with aqueous NaHCO3 (sat., 2×10 mL), brine (30 mL), and dried over anhydrous sodium sulfate. After the solvent was removed, the remaining oily residue was purified by a flash column chromatography to give 6. IR (film, cm−1) 3060, 3026, 2934, 2854, 2800, 2765, 1662, 1495, 1452, 1401, 1262, 1203, 1150, 1106, 966, 1033, 775, 749; LRMS 351.

후처리

  1. customAfter removal of the solvents
  2. customthe residue was dried under vacuum for 3 hrs
  3. dissolutionThe crude compound was dissolved in DMF (5.0 mL)
  4. stirringThe mixture was stirred at room temperature for 30 min
  5. stirringthe mixture was stirred at room temperature overnight
  6. customThe mixture was quenched with 10 mL of aqueous potassium carbonate (sat.)
  7. extractionextracted with ethyl acetate (3×60 mL)
  8. washwashed with aqueous NaHCO3 (sat., 2×10 mL), brine (30 mL)
  9. dry with materialdried over anhydrous sodium sulfate
  10. customAfter the solvent was removed
  11. customthe remaining oily residue was purified by a flash column chromatography
  12. customto give 6

출처 및 근거

ORD 기록
ord-e0feb61221144724bcea15c010535797
출처 데이터셋
uspto-grants-2004_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06677332B1

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트