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

HRID 21627

反応式

HRID 21627 の反応式
[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+].[CH3:25]I.Cl>CN(C)C=O.O>[CH3:25][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

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 863071,2-Dibenzoyl-1-(tert-butyl)hydrazine

生成物 1

HCID 15294607N-methyl-N'-t-butyl-N,N'-dibenzoylhydrazine

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

To a stirred solution of N'-t-butyl-N,N'-dibenzoylhydrazine (2.5 g, 0.008M) in dimethylformamide (DMF) (30 ml) at room temperature under nitrogen was added portionwise sodium hydride (60% oil dispersion) (0.4 g, 0.009M). The mixture was stirred at room temperature for 0.5 hours, and then methyl iodide (1.0 g, 0.008M) was added dropwise. The reaction mixture was allowed to stir for 1 hour. 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-methyl-N'-t-butyl-N,N'-dibenzoylhydrazine as an oil.

後処理

  1. stirringto stir for 1 hour
  2. extractionthe product extracted into methylene chloride (50 ml)
  3. washThe methylene chloride layer was washed with water (5×20 ml)
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customthe methylene chloride removed under vacuum

出典と根拠

ORDレコード
ord-35fc4fbb2cec488f98f20d76710491b4
出典データセット
uspto-grants-1995_06
特許番号
US05424333

関連ノート

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