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

Triethylamine → N'-(6-Chloro-5-(trimethylsilyl)pyridazin-3-yl)-2-fluorobenzohydrazide

HRID 1887032
노트
인쇄 미리보기

반응식

HRID 1887032 반응식
[Cl:1][C:2]1[N:3]=[N:4][C:5]([NH:12][NH2:13])=[CH:6][C:7]=1[Si:8]([CH3:11])([CH3:10])[CH3:9].C(N(CC)CC)C.[F:21][C:22]1[CH:30]=[CH:29][CH:28]=[CH:27][C:23]=1[C:24](Cl)=[O:25]>C(OCC)C>[Cl:1][C:2]1[N:3]=[N:4][C:5]([NH:12][NH:13][C:24](=[O:25])[C:23]2[CH:27]=[CH:28][CH:29]=[CH:30][C:22]=2[F:21])=[CH:6][C:7]=1[Si:8]([CH3:9])([CH3:10])[CH3:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 98082-Fluorobenzoyl chlorideHCID 154861653-Chloro-6-hydrazinyl-4-(trimethylsilyl)pyridazine

생성물 1

HCID 15486174N'-(6-Chloro-5-(trimethylsilyl)pyridazin-3-yl)-2-fluorobenzohydrazide수율 51.7%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

A solution of 21 (6.45 g, 30 mmol) and triethylamine (5 mL, 36 mmol) in diethyl ether (120 mL) was cooled to 0-5° C. in an ice bath. 2-Fluorobenzoyl chloride (4.8 g, 30 mmol) was added dropwise keeping the temperature less than 5° C. The reaction was stirred 30 min then quenched by the addition of anhydrous MeOH (0.4 mL). The mixture was diluted with hexane (100 mL) and filtered. The solids were washed with ether (2×15 mL), then water (30 mL). The solids were dissolved in dichloromethane (100 mL) with a small amount of MeOH to aid solubility, then washed with brine. The organic solution was dried over Na2SO4 and concentrated to give a 51.7% yield of 22 as a brownish solid.

후처리

  1. customthe temperature less than 5° C
  2. customthen quenched by the addition of anhydrous MeOH (0.4 mL)
  3. additionThe mixture was diluted with hexane (100 mL)
  4. filtrationfiltered
  5. washThe solids were washed with ether (2×15 mL)
  6. dissolutionThe solids were dissolved in dichloromethane (100 mL) with a small amount of MeOH
  7. washwashed with brine
  8. dry with materialThe organic solution was dried over Na2SO4
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-d34fd1bb6e3b4b41853a117f9f75731a
출처 데이터셋
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08501738B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트