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

Trifluoroacetic acid → Ethyl 4-{[2-(tert-butoxycarbonyl)-5-(4-methylpiperazin-1-yl)phenyl]amino}piperidine-1-carboxylate

HRID 1803862
노트
인쇄 미리보기

반응식

HRID 1803862 반응식
[NH2:1][C:2]1[CH:14]=[C:13]([N:15]2[CH2:20][CH2:19][N:18]([CH3:21])[CH2:17][CH2:16]2)[CH:12]=[CH:11][C:3]=1[C:4]([O:6][C:7]([CH3:10])([CH3:9])[CH3:8])=[O:5].[CH2:22]([O:24][C:25]([N:27]1[CH2:32][CH2:31][CH2:30][CH2:29][C:28]1=O)=[O:26])[CH3:23].FC(F)(F)C(O)=O.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C([O-])(O)=O.[Na+]>O1CCOCC1>[C:7]([O:6][C:4]([C:3]1[CH:11]=[CH:12][C:13]([N:15]2[CH2:20][CH2:19][N:18]([CH3:21])[CH2:17][CH2:16]2)=[CH:14][C:2]=1[NH:1][CH:30]1[CH2:31][CH2:32][N:27]([C:25]([O:24][CH2:22][CH3:23])=[O:26])[CH2:28][CH2:29]1)=[O:5])([CH3:10])([CH3:9])[CH3:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 6422Trifluoroacetic acidHCID 516892Sodium BicarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 13303317Ethyl 2-oxopiperidine-1-carboxylateHCID 667359202-Amino-4-(4-methylpiperazin-1-yl) benzoic acid tertbutyl ester

생성물 1

HCID 66996520
Ethyl 4-{[2-(tert-butoxycarbonyl)-5-(4-methylpiperazin-1-yl)phenyl]amino}piperidine-1-carboxylate
수율 95%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

tert-Butyl 2-amino-4-(4-methylpiperazin-1-yl)benzoate (1.5 g, 5.15 mmol) was dissolved in dry dioxane (25 mL) under a nitrogen atmosphere. N-ethoxycarbonylpiperidone (1.06 g, 0.932 mL, 6.18 mmol, 1.2 eq) was added, followed by trifluoroacetic acid (1.03 mL, 13.39 mmol, 2.6 eq) and sodium triacetoxyborohydride (1.72 g, 7.73 mmol, 1.5 eq). The mixture was stirred at room temperature for 4 hours. A saturated aqueous solution of NaHCO3 was then added, the mixture was concentrated under reduced pressure and extracted with dichloromethane (3×40 mL). The combined organic layers were washed with brine, dried over Na2SO4 and concentrated under reduced pressure. After purification by chromatography over silica gel (DCM/EtOH 93:7) 2.187 g of title compound were obtained as a white solid (95% yield).

후처리

  1. concentrationthe mixture was concentrated under reduced pressure
  2. extractionextracted with dichloromethane (3×40 mL)
  3. washThe combined organic layers were washed with brine
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated under reduced pressure
  6. customAfter purification by chromatography over silica gel (DCM/EtOH 93:7) 2.187 g of title compound

출처 및 근거

ORD 기록
ord-e3b1ca3bcd0a454aa0180526bbfe0fa7
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08354399B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트