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

1-Butanol → HCID 22320271, 화합물

HRID 497967
노트
인쇄 미리보기

반응식

HRID 497967 반응식
[CH2:1]([OH:5])[CH2:2][CH2:3][CH3:4].[H-].[Na+].Cl[C:9]1[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[N:12]=[C:11]2[N:19]([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][N:24]=3)[N:20]=[C:21]([CH3:22])[C:10]=12>O1CCCC1>[CH2:1]([O:5][C:9]1[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[N:12]=[C:11]2[N:19]([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][N:24]=3)[N:20]=[C:21]([CH3:22])[C:10]=12)[CH2:2][CH2:3][CH3:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 2631-ButanolHCID 24758Sodium hydrideHCID 223201094-Chloro-3-methyl-1-(2-pyridinyl)-1H-pyrazolo[3,4-b]quinoline

생성물 1

HCID 22320271HCID 22320271, 화합물수율 26%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To an ice-cold solution of 1-butanol (5.0 g, 68 mmol) in tetrahydrofuran (15 mL) was added sodium hydride (oiliness, content 60%, 0.41 g, 17 mmol), and the mixture was stirred at room temperature for 15 minutes. After 4-chloro-3-methyl-1-(2-pyridinyl)-1H-pyrazolo[3,4-b]quinoline (1.0 g, 3.39 mmol) was added thereto at 0° C., the mixture was heated under reflux further for 1 hour. The reaction mixture was allowed to cool to room temperature, and the solvent was evaporated and concentrated under reduced pressure. Iced water was added to the residue and the mixture was neutralized with dilute hydrochloric acid, and organic matter was extracted with ethyl acetate. The extract was washed with saturated brine and water, dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue thus obtained was purified by silica gel column chromatography (ethyl acetate) to give the title compound (0.29 g, 26% yield).

후처리

  1. temperatureat 0° C., the mixture was heated
  2. temperatureunder reflux further for 1 hour
  3. temperatureto cool to room temperature
  4. customthe solvent was evaporated
  5. concentrationconcentrated under reduced pressure
  6. additionIced water was added to the residue
  7. extractionwas extracted with ethyl acetate
  8. washThe extract was washed with saturated brine and water
  9. dry with materialdried over anhydrous magnesium sulfate
  10. customthe solvent was evaporated under reduced pressure
  11. customThe residue thus obtained
  12. customwas purified by silica gel column chromatography (ethyl acetate)

출처 및 근거

ORD 기록
ord-fd31ca305a5d4048b82b969d75455d51
출처 데이터셋
uspto-grants-2005_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06949648B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트