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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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2-Phenylhydrazinecarboxaldehyde → 1-methyl-2-phenylhydrazine

HRID 1952766
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HRID 1952766 반응식
[C:1]1([NH:7][NH:8][CH:9]=O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-]>O1CCCC1.CCOCC>[CH3:9][NH:8][NH:7][C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 121542-PhenylhydrazinecarboxaldehydeHCID 21226445Aluminium lithium hydride

생성물 1

HCID 101978131-methyl-2-phenylhydrazine수율 76.3%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of N'-phenylformohydrazide (20.59 g) in dry tetrahydrofuran (750 ml) was added dropwise under nitrogen to a stirred suspension of lithium aluminium hydride (10 g) in dry tetrahydrofuran (200 ml), then the mixture was stirred and heated under reflux for 4 hours. The mixture was quenched by the slow dropwise addition of water (10 ml), followed by 5M aqueous sodium hydroxide solution (10 ml), then water (20 ml), then it was filtered, dried (MgSO4) and the solvent removed in vacuo to yield an oil. The oil was dissolved in ether, redried (MgSO4) and the solvent removed in vacuo to yield 1-methyl-2-phenylhydrazine (14.1 g) as a yellow oil.

후처리

  1. temperatureheated
  2. temperatureunder reflux for 4 hours
  3. customThe mixture was quenched by the slow dropwise addition of water (10 ml)
  4. filtrationwater (20 ml), then it was filtered
  5. dry with materialdried (MgSO4)
  6. customthe solvent removed in vacuo
  7. customto yield an oil
  8. dry with materialredried (MgSO4)
  9. customthe solvent removed in vacuo

출처 및 근거

ORD 기록
ord-b7104568c8a149abbeed6e3faddea091
출처 데이터셋
uspto-grants-2000_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06114334

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