Sodium Hydroxide → HCID 86737146、化合物

HRID 1856123ノート

反応式

HRID 1856123 の反応式
Cl.[C:2]([NH:7][NH2:8])([CH2:5][CH3:6])([CH3:4])[CH3:3].[C:9]([O:16][CH2:17][CH:18]=[CH2:19])(=[O:15])[CH2:10][CH2:11][C:12]([CH3:14])=O.[OH-].[Na+]>O>[C:2]([NH:7][N:8]=[C:12]([CH3:14])[CH2:11][CH2:10][C:9]([O:16][CH2:17][CH:18]=[CH2:19])=[O:15])([CH2:5][CH3:6])([CH3:4])[CH3:3]

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 117545Hydrazine, (1,1-dimethylpropyl)-, monohydrochlorideHCID 529770Allyl 4-oxopentanoate

生成物 1

HCID 86737146HCID 86737146、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a 1 liter round bottom flask equipped with a magnetic stirrer and water-cooled condenser was added 760 grams (0.5 mole) of a 9.1% aqueous solution of t-amylhydrazine hydrochloride, 78 grams (0.5 mole) of allyl levulinate and 40 grams (0.5 mole) of 50% sodium hydroxide. The flask was placed in an oil bath on a magnetic stirrer and the contents stirred and heated to reflux. The reaction was refluxed gently for 3 hours and allowed to cool to room temperature. The organic layer was separated, dried over anhydrous sodium sulfate and the drying agent removed by filtration. The yellow liquid product weighed 116 grams (96.5% crude yield). The infrared spectrum of the product contained a strong band at 1718 cm-1 (carbonyl) and a weak band at 1620 cm-1 (C=N) indicating that the hydrazone band had formed and the ester group was still intact.

後処理

  1. customTo a 1 liter round bottom flask equipped with a magnetic stirrer
  2. customThe flask was placed in an oil bath on a magnetic stirrer
  3. temperatureheated to reflux
  4. temperatureThe reaction was refluxed gently for 3 hours
  5. customThe organic layer was separated
  6. dry with materialdried over anhydrous sodium sulfate
  7. customthe drying agent removed by filtration
  8. customhad formed

出典と根拠

ORDレコード
ord-0969b309a5064ee187ee7d70573bdfe9
出典データセット
uspto-grants-1980_08
特許番号
US04218370

反応ノート

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