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

Triethylamine → N,N-dimethyl-1-(2-nitro-4-(trifluoromethyl)phenyl)piperidin-4-amine

HRID 1042681
노트
인쇄 미리보기

반응식

HRID 1042681 반응식
Cl.Cl.C(N1CCC(N(C)C)CC1)C1C=CC=CC=1.Cl.Cl.[CH3:21][N:22]([CH3:29])[CH:23]1[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]1.F[C:31]1[CH:36]=[CH:35][C:34]([C:37]([F:40])([F:39])[F:38])=[CH:33][C:32]=1[N+:41]([O-:43])=[O:42].C(N(CC)CC)C>[Pd].O.C1COCC1.CO>[CH3:21][N:22]([CH3:29])[CH:23]1[CH2:28][CH2:27][N:26]([C:31]2[CH:36]=[CH:35][C:34]([C:37]([F:40])([F:38])[F:39])=[CH:33][C:32]=2[N+:41]([O-:43])=[O:42])[CH2:25][CH2:24]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 4

HCID 8471TriethylamineHCID 677784-Fluoro-3-nitrobenzotrifluorideHCID 225914404-(Dimethylamino)piperidine dihydrochlorideHCID 231533931-benzyl-N,N-dimethylpiperidin-4-amine dihydrochloride

생성물 1

HCID 16109041N,N-dimethyl-1-(2-nitro-4-(trifluoromethyl)phenyl)piperidin-4-amine

시약·촉매·용매 4

HCID 23938
Palladium
촉매
HCID 887Methanol용매
HCID 962Water용매
HCID 8028Tetrahydrofuran용매

실험 절차

To 1-benzyl-N,N-dimethylpiperidin-4-amine dihydrochloride (6.7 g, 23 mmol) was added Pd/C (10%, 2.4 g) under argon. Methanol (100 ml) was added via syringe, and H2 gas was introduced and the mixture stirred vigorously under an atmosphere of H2. After 48 h, the mixture was flushed with nitrogen, filtered through celite and concentrated to afford a mixture of starting material and N,N-dimethylpiperidin-4-amine dihydrochloride as a white solid. This solid was treated with 1-Fluoro-2-nitro-4-trifluoromethyl-benzene (3.2 ml, 22.9 mmol), triethylamine (12.7 ml, 92 mmol), and 50 ml dry THF. The mixture was heated to 75° C. with a water-cooled reflux condenser for 12 h. The mixture was allowed to cool to ambient temperature, was filtered through a fritted funnel, and concentrated to an orange oil. The residue was purified by silica gel chromatography (MC/MeOH/conc. NH4OH) to give the desired product as an orange oil. MS (m/z): 318.1 (M+H)+. Calc'd for C14H18F3N3O2: 317.31.

후처리

  1. additionH2 gas was introduced
  2. customthe mixture was flushed with nitrogen
  3. filtrationfiltered through celite
  4. concentrationconcentrated
  5. customto afford
  6. temperaturecooled
  7. temperaturereflux condenser for 12 h
  8. filtrationwas filtered through a fritted funnel
  9. concentrationconcentrated to an orange oil
  10. customThe residue was purified by silica gel chromatography (MC/MeOH/conc. NH4OH)

출처 및 근거

ORD 기록
ord-397d90546d184251ab9777be06ecdf5f
출처 데이터셋
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08557996B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트