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Benzene → N-(alpha,alpha-dimethylbenzyl)-alpha-bromo-isovaleramide

HRID 1680606
ノート
印刷プレビュー

反応式

HRID 1680606 の反応式
C1C=CC=CC=1.[CH3:7][C:8]([NH2:16])([CH3:15])[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.[Br:17][CH:18]([CH:22]([CH3:24])[CH3:23])[C:19](Cl)=[O:20]>C(N(CC)CC)C>[CH3:7][C:8]([NH:16][C:19](=[O:20])[CH:18]([Br:17])[CH:22]([CH3:24])[CH3:23])([CH3:15])[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 241BenzeneHCID 68509CumylamineHCID 124869822-Bromo-3-methylbutanoyl chloride

生成物 1

HCID 12895705N-(alpha,alpha-dimethylbenzyl)-alpha-bromo-isovaleramide収率 85.1%

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

Into a 200 ml four necked flask, there were charged benzene (100 ml), α,α-dimethylbenzylamine (9 g) and triethylamine (7.4 g), and α-bromo-isovaleryl chloride (13.3 g) was dropwise added thereto while stirring at room temperature. Stirring was continued for 3 hours. The reaction mixture was washed with water to remove triethylamine hydrochloride. After the benzene layer was dried over anhydrous sodium sulfate, the solvent was distilled off under reduced pressure. The obtained residue was recrystallized from ethanol to give 16.9 g of N-(α,α-dimethylbenzyl)-α-bromo-isovaleramide. M.P., 128°-129.5° C.

後処理

  1. additionwas dropwise added
  2. stirringStirring
  3. washThe reaction mixture was washed with water
  4. customto remove triethylamine hydrochloride
  5. dry with materialAfter the benzene layer was dried over anhydrous sodium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. customThe obtained residue was recrystallized from ethanol

出典と根拠

ORDレコード
ord-77804d46595a40bcb9f6de68d3b2d75c
出典データセット
uspto-grants-1981_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04274862

反応ノート

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