Toluene → HCID 12895677、化合物

HRID 1680605ノート

反応式

HRID 1680605 の反応式
C1(C)C=CC=CC=1.[CH3:8][C:9]([NH2:17])([CH3:16])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.[CH3:18][CH:19]([C:23]([CH3:26])([CH3:25])[CH3:24])[C:20](Cl)=[O:21]>N1C=CC=CC=1>[CH3:8][C:9]([NH:17][C:20](=[O:21])[CH:19]([C:23]([CH3:26])([CH3:25])[CH3:24])[CH3:18])([CH3:16])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

参加物

5

反応物 3

HCID 1140TolueneHCID 68509CumylamineHCID 125476452,3,3-Trimethylbutanoyl chloride

生成物 1

HCID 12895677HCID 12895677、化合物収率 83.8%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

Into a 200 ml four-necked flask, there were charged toluene (100 ml), α,α-dimethylbenzylamine (9 g) and pyridine (5.8 g), and α-methyl-tert-butylacetyl chloride (9.9 g) was dropwise added thereto while stirring at room temperature. Stirring was continuted for 3 hours. The reaction mixture was washed with water to remove pyridine hydrochloride. After the toluene layer was dried over anhydrous sodium sulfate, the solvent was distilled off under reduced pressure. The obtained residue was recrystallized from ethanol to give 13.8 g of N-(α,α-dimethylbenzyl)-α-methyl-tert-butylacetamide. M.P., 162.5°-163.5° C.

後処理

  1. additionwas dropwise added
  2. stirringStirring
  3. washThe reaction mixture was washed with water
  4. customto remove pyridine hydrochloride
  5. dry with materialAfter the toluene 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-94f27b1ee03b47cfa62cea969e3c4312
出典データセット
uspto-grants-1981_06
特許番号
US04274862

反応ノート

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