Hydrochloric Acid → N-allyl-N'-t-butyl-N,N'-dibenzoylhydrazine

HRID 21629

반응식

HRID 21629 반응식
[C:1]([N:5]([C:15](=[O:22])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)[NH:6][C:7](=[O:14])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)([CH3:4])([CH3:3])[CH3:2].[H-].[Na+].[CH2:25](I)[CH:26]=[CH2:27].Cl>CN(C=O)C.O>[CH2:27]([N:6]([C:7](=[O:14])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[N:5]([C:1]([CH3:4])([CH3:2])[CH3:3])[C:15](=[O:22])[C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1)[CH:26]=[CH2:25]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 11166Allyl iodideHCID 24758Sodium hydrideHCID 863071,2-Dibenzoyl-1-(tert-butyl)hydrazine

생성물 1

HCID 15294608N-allyl-N'-t-butyl-N,N'-dibenzoylhydrazine

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

To a stirred solution of N'-t-butyl-N,N'-dibenzoylhydrazine (3 g, 0.011M) in DMF (30 ml) at room temperature under nitrogen was added portionwise sodium hydride (60% oil dispersion) (0.5 g, 0.012M). The mixture was stirred at room temperature for 0.5 hours, and then allyl iodide (1.8 g, 0.01M) was added dropwise. The reaction mixture was warmed to 60° C. and stirred for 2 hours. The mixture was then diluted with water (50 ml), neutralized with 10% HCl and the product extracted into methylene chloride (50 ml). The methylene chloride layer was washed with water (5×20 ml), dried over anhydrous magnesium sulfate and the methylene chloride removed under vacuum to afford N-allyl-N'-t-butyl-N,N'-dibenzoylhydrazine as an oil.

후처리

  1. temperatureThe reaction mixture was warmed to 60° C.
  2. stirringstirred for 2 hours
  3. extractionthe product extracted into methylene chloride (50 ml)
  4. washThe methylene chloride layer was washed with water (5×20 ml)
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customthe methylene chloride removed under vacuum

출처 및 근거

ORD 기록
ord-1f565d8e745b4d0f90d3eefa8cd0e70b
출처 데이터셋
uspto-grants-1995_06
특허 번호
US05424333

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