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

Triethylamine → 1-(2,6-Difluoro-4-nitrophenyl)piperidin-4-one

HRID 1512153
노트
인쇄 미리보기

반응식

HRID 1512153 반응식
[F:1][C:2]1[CH:3]=[C:4]([N+:10]([O-:12])=[O:11])[CH:5]=[C:6]([F:9])[C:7]=1F.O.Cl.[NH:15]1[CH2:20][CH2:19][C:18](=[O:21])[CH2:17][CH2:16]1.C(N(CC)CC)C>C(Cl)(Cl)Cl>[F:9][C:6]1[CH:5]=[C:4]([N+:10]([O-:12])=[O:11])[CH:3]=[C:2]([F:1])[C:7]=1[N:15]1[CH2:20][CH2:19][C:18](=[O:21])[CH2:17][CH2:16]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 2723901PiperonylamineHCID 27827931,2,3-Trifluoro-5-nitrobenzene

생성물 1

HCID 218781831-(2,6-Difluoro-4-nitrophenyl)piperidin-4-one수율 94%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

To a mixture of 3,4,5-trifluoronitrobenzene (3.894 g, 0.022 mol) and 4-piperidone hydrochloride monohydrate (3.072 g, 0.020 mol) in chloroform (24 ml), was added triethylamine (8.3 ml, 0.06 mol) under stirring. The resulting mixture was heated and stirred at 70° C. for 7 h. After completion of the reaction (TLC), the solvent was evaporated under reduced pressure and the residue diluted with water (10 ml). The separated solid was filtered, washed with water (8 ml) followed by hexane (5 ml) to obtain yellow crystalline solid as a product, 4.8 g, 94% yield M.P.: 130-132° C.; MS: M+1=257 (MH+ 100%) for M.F.: C11H10F2N2O3

후처리

  1. temperatureThe resulting mixture was heated
  2. stirringstirred at 70° C. for 7 h
  3. customAfter completion of the reaction (TLC)
  4. customthe solvent was evaporated under reduced pressure
  5. additionthe residue diluted with water (10 ml)
  6. filtrationThe separated solid was filtered
  7. washwashed with water (8 ml)
  8. customto obtain yellow crystalline solid as a product

출처 및 근거

ORD 기록
ord-fa38bc2ed7aa4e96a0d24a7e09bb80a9
출처 데이터셋
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08217058B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트