Benzene → Bromobutide

HRID 1577467

反応式

HRID 1577467 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]([C:22]([CH3:25])([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]([C:22]([CH3:25])([CH3:24])[CH3:23])[Br:17])([CH3:15])[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1

参加物

5

反応物 3

HCID 241BenzeneHCID 68509CumylamineHCID 108676212-Bromo-3,3-dimethylbutanoyl chloride

生成物 1

HCID 53079Bromobutide収率 73.6%

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-tert-butylacetyl chloride (14.5 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 15.3 g of N-(α,α-dimethylbenzyl)-α-bromo-tert-butylacetamide. M.P., 182°-183° 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-6533c47c46e047fead1c18a1f7f5fbfb
出典データセット
uspto-grants-1981_09
特許番号
US04288244

関連ノート

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