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

1,8-Diazabicyclo(5.4.0)undec-7-ene → 7-Amino-5-[4-(2-[7-amino-2-(2-furyl)-[1,2,4]triazolo[1,5-a][1,3,5]triazin-5-ylamino]ethyl)phenoxy]-2-(2-furyl)[1,2,4]triazolo[1,5-a][1,3,5]triazine

HRID 5819
노트
인쇄 미리보기

반응식

HRID 5819 반응식
[NH2:1][C:2]1[N:7]2[N:8]=[C:9]([C:11]3[O:12][CH:13]=[CH:14][CH:15]=3)[N:10]=[C:6]2[N:5]=[C:4]([NH:16][CH2:17][CH2:18][C:19]2[CH:24]=[CH:23][C:22]([OH:25])=[CH:21][CH:20]=2)[N:3]=1.N12CCCN=C1CCCCC2.[NH2:37][C:38]1[N:43]2[N:44]=[C:45]([C:47]3[O:48][CH:49]=[CH:50][CH:51]=3)[N:46]=[C:42]2[N:41]=[C:40](S(C)(=O)=O)[N:39]=1.C(Cl)Cl.CO>C(#N)C>[NH2:37][C:38]1[N:43]2[N:44]=[C:45]([C:47]3[O:48][CH:49]=[CH:50][CH:51]=3)[N:46]=[C:42]2[N:41]=[C:40]([O:25][C:22]2[CH:21]=[CH:20][C:19]([CH2:18][CH2:17][NH:16][C:4]3[N:3]=[C:2]([NH2:1])[N:7]4[N:8]=[C:9]([C:11]5[O:12][CH:13]=[CH:14][CH:15]=5)[N:10]=[C:6]4[N:5]=3)=[CH:24][CH:23]=2)[N:39]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 1764074-(2-(7-Amino-2-(2-furyl)-(1,2,4)triazolo(2,3-a)-(1,3,5)triazin-5-yl-amino)ethyl)phenolHCID 99708822-(Furan-2-yl)-5-(methylsulfonyl)-[1,2,4]triazolo[1,5-a][1,3,5]triazin-7-amineHCID 21226129Dichloromethane methanol

생성물 1

HCID 9871898
7-Amino-5-[4-(2-[7-amino-2-(2-furyl)-[1,2,4]triazolo[1,5-a][1,3,5]triazin-5-ylamino]ethyl)phenoxy]-2-(2-furyl)[1,2,4]triazolo[1,5-a][1,3,5]triazine

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

7-amino-2-(2-furyl)-5-[2-(4-hydroxyphenyl)ethyl]amino[1,2,4]-triazolo[1,5-a][1,3,5]triazine (0.91 g) and 1,8-diazabicyclo[5,4,0]undec-7-ene (DBU, 0.37 ml) were added to a suspension of 7-amino-2-(2-furyl)-5-methylsulphonyl-[1,2,4]triazolo[1,5-a][1,3,5]triazine (0.82 g) in acetonitrile (50 ml) and the resulting mixture was heated under reflux for 17 hours, after which time thin layer chromatography (TLC) analysis on silica plates (eluent: methylene chloride-methanol 19:1 v/v) indicated that no methanesulphonyl starting material remained. The solvent was then evaporated and the residue was purified by column chromatography on silica (75 g) eluting with ethyl acetate-methylene chloride 7:3 v/v. A white solid was obtained, and this was crystallised from isopropanol to afford 7-amino-5-[4-(2-[7-amino-2-(2-furyl)-[1,2,4]triazolo[1,5-a][1,3,5]triazin-5-ylamino]ethyl)phenoxy]-2-(2-furyl)[ 1,2,4]triazolo[1,5-a][1,3,5]triazine, m.p. 285°-289° C.; microanalysis, found: C, 54.1; H, 4.4; N, 30.8%; C24H19N13O3 1.0(C3H7OH) requires: C, 54.2; H, 4.5; N, 30.5%; NMR: 2.92 (t, 2H, phenyl-CH2), 3.55 (q, 2H, CH2-N), 6.67 (m, 2H, 2 furyl-4H), 7.0 (d, 1H, furyl-3H), 7.11 (d, 1H, furyl-3'H), 7.16 and 7.35 (A2B2 pattern, 4H, phenyl-H), 7.5 (br t, 1H, NH rotamers), 7.85 (d, 1H, furyl-5H), 7.89 (d, 1H, furyl-5'H), 8.12 (br s, 2H, NH2) and 8.93 (d, 2H, NH2); m/e (M+H)+ 538.

후처리

  1. temperaturethe resulting mixture was heated
  2. temperatureunder reflux for 17 hours
  3. customThe solvent was then evaporated
  4. customthe residue was purified by column chromatography on silica (75 g)
  5. washeluting with ethyl acetate-methylene chloride 7:3 v/v
  6. customA white solid was obtained
  7. customthis was crystallised from isopropanol

출처 및 근거

ORD 기록
ord-a3390456313144aa978257dac6d1ec7e
출처 데이터셋
uspto-grants-1993_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05246932

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트