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Methyl Isobutyl Ketone → N-(alpha,alpha-dimethylbenzyl)-alpha-bromo-isovaleramide

HRID 1680607
ノート
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反応式

HRID 1680607 の反応式
CC(CC(C)C)=O.[CH3:8][C:9]([NH2:17])([CH3:16])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.C(N(CC)CC)C.[Br:25][CH:26]([CH:30]([CH3:32])[CH3:31])[C:27](Cl)=[O:28]>O>[CH3:8][C:9]([NH:17][C:27](=[O:28])[CH:26]([Br:25])[CH:30]([CH3:32])[CH3:31])([CH3:16])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 7909Methyl Isobutyl KetoneHCID 8471TriethylamineHCID 68509CumylamineHCID 124869822-Bromo-3-methylbutanoyl chloride

生成物 1

HCID 12895705N-(alpha,alpha-dimethylbenzyl)-alpha-bromo-isovaleramide収率 87.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Into a 500 ml four-necked flask, there were charged methylisobutylketone (150 ml), α,α-dimethylbenzylamine (27.0 g) and triethylamine (21.2 g), and α-bromo-isovaleryl chloride (40.0 g) was dropwise added thereto while stirring at room temperature. Stirring was continued for 3 hours. After completion of the reaction, water (200 ml) was added thereto and the reaction mixture was gradually heated to remove methylisobutylketone, followed by cooling at room temperature. The precipitated crystals were filtered, washed with water, dried and recrystallized from ethanol to give N-(α,α-dimethylbenzyl)-α-bromo-isovaleramide (51.9 g).

後処理

  1. additionwas dropwise added
  2. stirringStirring
  3. additionwas added
  4. temperaturethe reaction mixture was gradually heated
  5. customto remove methylisobutylketone
  6. temperatureby cooling at room temperature
  7. filtrationThe precipitated crystals were filtered
  8. washwashed with water
  9. customdried
  10. customrecrystallized from ethanol

出典と根拠

ORDレコード
ord-2da2347d7f1e4112801853393bc0520d
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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