3-Cyano-4-isobutoxyaniline hydrochloride → 3-Cyano-4-isobutoxy-phenylhydrazine

HRID 850063노트

반응식

HRID 850063 반응식
Cl.[C:2]([C:4]1[CH:5]=[C:6]([CH:8]=[CH:9][C:10]=1[O:11][CH2:12][CH:13]([CH3:15])[CH3:14])[NH2:7])#[N:3].[N:16]([O-])=O.[Na+]>>[C:2]([C:4]1[CH:5]=[C:6]([NH:7][NH2:16])[CH:8]=[CH:9][C:10]=1[O:11][CH2:12][CH:13]([CH3:15])[CH3:14])#[N:3]

참가 물질

3

반응물 2

HCID 193660273-Cyano-4-isobutoxyaniline hydrochlorideHCID 23668193Sodium Nitrite

생성물 1

HCID 154065483-Cyano-4-isobutoxy-phenylhydrazine수율 82.8%

실험 절차

To an aqueous solution (34 ml) of 3-cyano-4-isobutoxyaniline hydrochloride (20 g) were added sodium nitrite (6.8 g), stannous chloride dihydrate (61 g) and con. hydrochloric add (100 ml) with stirring under ice-cooling. After the completion of the reaction, precipitated crystals were collected by filtration. The crystals were added to water, and the mixture was neutralized with aqueous sodium hydroxide solution, extracted with a mixed solvent of toluene and tert-butanol, washed with water and dried over magnesium sulfate. The solvent was evaporated under reduced pressure to give 15 g of 3-cyano-4-isobutoxy-phenylhydrazine.

후처리

  1. additionhydrochloric add (100 ml)
  2. temperaturecooling
  3. customAfter the completion of the reaction
  4. customprecipitated crystals
  5. filtrationwere collected by filtration
  6. additionThe crystals were added to water
  7. extractionextracted with a mixed solvent of toluene and tert-butanol
  8. washwashed with water
  9. dry with materialdried over magnesium sulfate
  10. customThe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-7930b7ff2d62446faaf6dfcd2c408bfc
출처 데이터셋
uspto-grants-2000_01
특허 번호
US06015829

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