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

Water → 1,1-Dimethyl-2-(3-pyridylmethyl)hydrazine

HRID 1584994
노트
인쇄 미리보기

반응식

HRID 1584994 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][N:8]([CH3:17])[N:9]=[CH:10][C:11]1[CH:12]=[N:13][CH:14]=[CH:15][CH:16]=1.O.[OH-].[Na+]>C(OCC)C>[CH3:7][N:8]([CH3:17])[NH:9][CH2:10][C:11]1[CH:12]=[N:13][CH:14]=[CH:15][CH:16]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 311921Nicotinaldehyde dimethylhydrazoneHCID 21226445Aluminium lithium hydride

생성물 1

HCID 111481501,1-Dimethyl-2-(3-pyridylmethyl)hydrazine수율 20.6%

시약·촉매·용매 1

HCID 3283Diethyl Ether
용매
2회

반응 조건

온도
5 °C

실험 절차

In 100 ml of dry ethyl ether was suspended 4.6 g of lithium aluminum hydride and with stirring in a nitrogen gas stream, a solution of 12.0 g of 1,1-dimethyl-2-(3-pyridylmethylidene)hydrazine in 50 ml of dry ethyl ether was added dropwise. The mixture was refluxed For 5 hours and, then, cooled (5° C.) and with stirring, 5 ml of water, 5 ml of 20% aqueous sodium hydroxide and 15 ml of water were added dropwise in succession. The insoluble matter was filtered off, the filtrate was concentrated, and the residue was purified by silica gel column chromatography (eluent: chloroformethanol=10:1). The resulting oil was distilled under reduced pressure to give 2.5 g of the title compound as a yellow oil.

후처리

  1. temperatureThe mixture was refluxed For 5 hours
  2. stirringwith stirring
  3. filtrationThe insoluble matter was filtered off
  4. concentrationthe filtrate was concentrated
  5. customthe residue was purified by silica gel column chromatography (eluent: chloroformethanol=10:1)
  6. distillationThe resulting oil was distilled under reduced pressure

출처 및 근거

ORD 기록
ord-b8f16b45e7594daa83879cbeb4b13216
출처 데이터셋
uspto-grants-1999_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05935981

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트