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

1-benzyl-4-methylenepiperidine → HCID 68587687, 화합물

HRID 2070893
노트
인쇄 미리보기

반응식

HRID 2070893 반응식
[CH2:1]([N:3]1[CH2:8][CH2:7][CH:6]([CH2:9][C:10]2[N:15]3[N:16]=[C:17]([NH:19][C:20]4[CH:25]=[CH:24][C:23]([C:26]([F:29])([F:28])[F:27])=[CH:22][CH:21]=4)[N:18]=[C:14]3[CH:13]=[CH:12][CH:11]=2)[CH2:5][CH2:4]1)[CH3:2].C(N1CCC(=C)CC1)C1C=CC=CC=1.Br[C:45]1[N:50]2[N:51]=[C:52]([NH:54][C:55]3[CH:60]=[CH:59][C:58]([C:61]([F:64])([F:63])[F:62])=[CH:57][CH:56]=3)[N:53]=[C:49]2[CH:48]=[CH:47][CH:46]=1.C1(NC2N=C3C=CC=C(CC4CCNCC4)N3N=2)C=CC=CC=1.C(N1CCC(CC2N3N=C(NC4C=CC(C(F)(F)F)=CC=4)N=C3C=CC=2)CC1)C1C=CC=CC=1.N1CCC(CC2N3N=C(NC4C=CC(C(F)(F)F)=CC=4)N=C3C=CC=2)CC1>C(O)C.[Pd].C(O)(=O)C>[CH2:1]([N:3]1[CH2:4][CH2:5][CH:6]([CH2:9][C:10]2[N:15]3[N:16]=[C:17]([NH:19][C:20]4[CH:21]=[CH:22][C:23]([C:26]([F:28])([F:27])[F:29])=[CH:24][CH:25]=4)[N:18]=[C:14]3[CH:13]=[CH:12][CH:11]=2)[CH2:7][CH2:8]1)[CH3:2].[F:64][C:61]([F:62])([F:63])[C:58]1[CH:59]=[CH:60][C:55]([NH:54][C:52]2[N:53]=[C:49]3[CH:48]=[CH:47][CH:46]=[CH:45][N:50]3[N:51]=2)=[CH:56][CH:57]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

11

반응물 6

HCID 38261121-benzyl-4-methylenepiperidineHCID 59276367HCID 59276367, 화합물HCID 59276484HCID 59276484, 화합물HCID 59276502HCID 59276502, 화합물HCID 70921800HCID 70921800, 화합물HCID 86675554HCID 86675554, 화합물

생성물 2

HCID 59276484
HCID 59276484, 화합물
HCID 68587687HCID 68587687, 화합물수율 13.29%

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 176Acetic Acid용매HCID 702Ethanol용매

실험 절차

5-((1-Ethylpiperidin-4-yl)methyl)-N-(4-(trifluoromethyl)phenyl)-[1,2,4]triazolo[1,5-a]pyridin-2-amine. 541-Benzylpiperidin-4-yl)methyl)-N-(4-(trifluoromethyl)phenyl)-[1,2,4]triazolo[1,5-a]pyridin-2-amine was synthesized from 1-benzyl-4-methylenepiperidine and 5-bromo-N-(4-(trifluoromethyl)phenyl)-[1,2,4]triazolo[1,5-a]pyridin-2-amine following the procedure described for N-phenyl-5-(piperidin-4-ylmethyl)-[1,2,4]triazolo[1,5-a]pyridin-2-amine. 5-((1-Benzylpiperidin-4-yl)methyl)-N-(4-(trifluoromethyl)phenyl)-[1,2,4]triazolo[1,5-a]pyridin-2-amine (0.165 g, 0.354 mmol) was dissolved in ethanol (30 mL) and treated with a catalytic amount of palladium on carbon (10 weight %). The reaction was stirred under an atmosphere of hydrogen gas overnight at room temperature. As only trace conversion was observed, a drop of acetic acid was added and the reaction was stirred at room temperature overnight. Most of the starting material was converted to the title compound contaminated with a minor amount of 5-(piperidin-4-ylmethyl)-N-(4-(trifluoromethyl)phenyl)-[1,2,4]triazolo[1,5-a]pyridin-2-amine. The catalyst was removed by filtration washed with methanol and the filtrate was concentrated under reduced pressure. The residue was purified by semi-preparative HPLC (20-70% acetonitrile+0.1% trifluoroacetic acid in water+0.1% trifluoroacetic acid, 3 injections, 30 min.). The desired fractions were combined and neutralized with a STRATA cationic resin exchange column. The eluate was concentrated under reduced pressure and dried in a vacuum oven for 5 h. 541-Ethylpiperidin-4-yl)methyl)-N-(4-(trifluoromethyl)phenyl)-[1,2,4]triazolo[1,5-a]pyridin-2-amine (0.019 g, 0.047 mmol, 13.29% yield) was isolated as a off-white solid. 1H NMR (400 MHz, DMSO-d6) δ (ppm) 10.18 (s, 1H), 7.91 (d, J=8.59 Hz, 2H), 7.64 (d, J=8.59 Hz, 2H), 7.48-7.59 (m, 2H), 6.95 (s, 1H), 3.03 (d, J=6.64 Hz, 2H), 2.82 (br s, 2H), 2.26 (s, 2H), 1.99 (br s, 1H), 1.78 (br s, 2H), 1.55 (br s, 2H), 1.33 (br s, 2H), 0.89-1.02 (m, 3H); 19F NMR (400 MHz, DMSO-d6) δ (ppm)-59.9 ppm; MS (ESI): m/z 404.2 [M+1]+.

후처리

  1. stirringthe reaction was stirred at room temperature overnight
  2. customThe catalyst was removed by filtration
  3. washwashed with methanol
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customThe residue was purified by semi-preparative HPLC (20-70% acetonitrile+0.1% trifluoroacetic acid in water+0.1% trifluoroacetic acid, 3 injections, 30 min.)
  6. concentrationThe eluate was concentrated under reduced pressure
  7. customdried in a vacuum oven for 5 h

출처 및 근거

ORD 기록
ord-74cb1cd09c554421a2adbceb703f7a88
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08299056B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트