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

Diethyl Ether → Imidazo[1,2-d][1,2,4]triazin-8(7H)-one

HRID 1723676
노트
인쇄 미리보기

반응식

HRID 1723676 반응식
[NH:1]([C:3]([C:5]1[NH:6][CH:7]=[CH:8][N:9]=1)=[O:4])[NH2:2].[CH3:10]OC(OC)N(C)C.C(OCC)C>C1C=CC(C2C=CC=CC=2)=CC=1.C1C=CC(OC2C=CC=CC=2)=CC=1>[N:6]1[CH:7]=[CH:8][N:9]2[C:5]=1[C:3](=[O:4])[NH:1][N:2]=[CH:10]2
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 78373Dimethylformamide dimethyl acetalHCID 12493320HCID 12493320, 화합물

생성물 1

HCID 45087660Imidazo[1,2-d][1,2,4]triazin-8(7H)-one수율 20%

시약·촉매·용매 1

HCID 246701,1'-Biphenyl, mixt. with 1,1'-oxybis(benzene)용매

반응 조건

온도
100 °C

실험 절차

2-Hydrazinocarbonylimidazole (prepared according to the procedure described in EP-A-0713876) (1.00 g, 7.93 mmol) was suspended in Dowtherm A (6 ml), N,N-dimethylformamide dimethyl acetal (1.89 g, 15.9 mmol) added and the mixture heated at 100° C. for 1.5 h then at 210° C. for 18 h. The mixture was allowed to cool to room temperature, diethyl ether (100 ml) added and the precipitated solid was filtered. The brown solid was purified by dry flash column chromatography on silica eluting with dichloromethane (+0.1% 0.880 ammonia) on a gradient of methanol (5-12%). Collecting appropriate fractions gave 7H-imidazo[1,2-d][1,2,4]triazin-8-one (216 mg, 20%) as an off-white solid: δH (400 MHz, CDCl3) 7.59 (1H, d, J 1), 7.91 (1H, d, J 1), 8.74 (1H, s), 12.39 (1H, s).

후처리

  1. temperatureto cool to room temperature
  2. filtrationthe precipitated solid was filtered
  3. customThe brown solid was purified
  4. dry with materialby dry flash column chromatography on silica eluting with dichloromethane (+0.1% 0.880 ammonia) on a gradient of methanol (5-12%)
  5. customCollecting appropriate fractions

출처 및 근거

ORD 기록
ord-0811cb2b9fbd49c896131525de938986
출처 데이터셋
uspto-grants-2009_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07485640B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트