Sodium Hydroxide → HCID 86737146, 화합물

HRID 1856123노트

반응식

HRID 1856123 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 86737146HCID 86737146, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0969b309a5064ee187ee7d70573bdfe9
출처 데이터셋
uspto-grants-1980_08
특허 번호
US04218370

반응 노트

불러오는 중…