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

Sodium hydride → 3-(2,5-Difluorophenyl)-7-(1,1-dimethylethyl)-6-((1-methyl-1H-1,2,4-triazol-5-yl)methoxy)-1,2,4-triazolo(4,3-b)pyridazine

HRID 2301336
노트
인쇄 미리보기

반응식

HRID 2301336 반응식
[CH3:1][N:2]1[C:6]([CH2:7][OH:8])=[N:5][CH:4]=[N:3]1.Cl[C:10]1[C:11]([C:27]([CH3:30])([CH3:29])[CH3:28])=[CH:12][C:13]2[N:14]([C:16]([C:19]3[CH:24]=[C:23]([F:25])[CH:22]=[CH:21][C:20]=3[F:26])=[N:17][N:18]=2)[N:15]=1.[H-].[Na+]>CN(C=O)C.O>[F:26][C:20]1[CH:21]=[CH:22][C:23]([F:25])=[CH:24][C:19]=1[C:16]1[N:14]2[N:15]=[C:10]([O:8][CH2:7][C:6]3[N:2]([CH3:1])[N:3]=[CH:4][N:5]=3)[C:11]([C:27]([CH3:30])([CH3:29])[CH3:28])=[CH:12][C:13]2=[N:18][N:17]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 24758Sodium hydrideHCID 11073377(1-methyl-1H-1,2,4-triazol-5-yl)methanolHCID 112557487-tert-Butyl-6-chloro-3-(2,5-difluorophenyl)-1,2,4-triazolo[4,3-b]pyridazine

생성물 1

HCID 99088803-(2,5-Difluorophenyl)-7-(1,1-dimethylethyl)-6-((1-methyl-1H-1,2,4-triazol-5-yl)methoxy)-1,2,4-triazolo(4,3-b)pyridazine수율 71.1%

시약·촉매·용매 2

HCID 962
Water
용매
HCID 6228Dimethylformamide용매

실험 절차

To a solution of (2-methyl-2H-1,2,4-triazol-3-yl)methanol (0.069 g, 0.4 mmol) and 6-chloro-3-(2,5-difluorophenyl)-7-(1,1-dimethylethyl)-1,2,4-triazolo[4,3-b]pyridazine (0.10 g, 0.31 mmol) in DMF (10 ml) was added sodium hydride (0.015 g of a 60% dispersion in oil, 1.2 mol eq.) and the reaction mixture was stirred at room temperature for 40 minutes. After this time the reaction mixture was diluted with water (80 ml) and the solid that precipitated was collected by filtration and washed several times with water in the sinter funnel. The solid was recrystallised from ethyl acetate/hexane to give pure title compound (0.088 g, 65%). Data for the title compound: 1H NMR (360 MHz, CDCl3) δ1.41 (9H, s), 3.89 (3H, s), 5.54 (2H, s), 7.23-7.26 (2H, m), 7.64 (1H, m), 7.91 (1H, s), 8.00 (1H, s); MS (ES+) m/e 400 [MH]+. Anal. Found C, 57.36; H, 4.61; N, 24.60%. C19H19F2N7O requires C, 57.14; H, 4.79; N, 24.55%.

후처리

  1. customthe solid that precipitated
  2. filtrationwas collected by filtration
  3. washwashed several times with water in the sinter funnel
  4. customThe solid was recrystallised from ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-510126639d504680a5fe74d968f2ef9c
출처 데이터셋
uspto-grants-2002_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06500828B1

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트