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

Hydrazine hydrate (1:1) → HCID 58951926, 화합물

HRID 1694797
노트
인쇄 미리보기

반응식

HRID 1694797 반응식
[CH2:1]([N:8]1[C:12]([CH2:13][CH:14]([C:19](=O)[CH2:20][CH3:21])[C:15](=O)[CH2:16][CH3:17])=[CH:11][N:10]=[CH:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.[NH2:24][NH2:25]>C(O)C>[CH2:1]([N:8]1[C:12]([CH2:13][C:14]2[C:19]([CH2:20][CH3:21])=[N:24][NH:25][C:15]=2[CH2:16][CH3:17])=[CH:11][N:10]=[CH:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 58951913HCID 58951913, 화합물

생성물 1

HCID 58951926HCID 58951926, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

To a solution of 140 mg (0.47 mmol) 4-(3-benzyl-3H-imidazol-4-ylmethyl)-heptane-3,5-dione in 1.5 ml ethanol was added a solution of 24 mg (0.48 mmol) hydrazine monohydrate in 0.5 ml ethanol and the mixture heated to reflux for 10 min. The reaction mixture was evaporated under reduced pressure, the residue dissolved in 1N aqueous HCl solution and extracted three times with t-butyl methyl ether. The aqueous phase was adjusted to pH 12 and extracted three times with t-butyl methyl ether, the combined extracts washed with brine, dried over sodium sulfate, filtered and evaporated. Purification of the residue by flash-chromatography on silica gel with ethyl acetate as eluent provided 4-(3-benzyl-3H-imidazol-4-ylmethyl)-3,5-diethyl-1H-pyrazole as colourless viscous oil: MS (ISP): 295.3 ((M+H)+.).

후처리

  1. temperaturethe mixture heated
  2. temperatureto reflux for 10 min
  3. customThe reaction mixture was evaporated under reduced pressure
  4. dissolutionthe residue dissolved in 1N aqueous HCl solution
  5. extractionextracted three times with t-butyl methyl ether
  6. extractionextracted three times with t-butyl methyl ether
  7. washthe combined extracts washed with brine
  8. dry with materialdried over sodium sulfate
  9. filtrationfiltered
  10. customevaporated
  11. customPurification of the residue by flash-chromatography on silica gel with ethyl acetate as eluent

출처 및 근거

ORD 기록
ord-1b65ab00651b4e9abb7bfc0209c0ead3
출처 데이터셋
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08158668B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트