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

HRID 850063ノート

反応式

HRID 850063 の反応式
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]

参加物

3

反応物 2

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

生成物 1

HCID 154065483-Cyano-4-isobutoxy-phenylhydrazine収率 82.8%

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7930b7ff2d62446faaf6dfcd2c408bfc
出典データセット
uspto-grants-2000_01
特許番号
US06015829

反応ノート

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