Methyl Isobutyl Ketone → Bromobutide

HRID 1577468

反応式

HRID 1577468 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]([C:30]([CH3:33])([CH3:32])[CH3:31])[C:27](Br)=[O:28]>O>[CH3:8][C:9]([NH:17][C:27](=[O:28])[CH:26]([C:30]([CH3:33])([CH3:32])[CH3:31])[Br:25])([CH3:16])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

参加物

6

反応物 4

HCID 7909Methyl Isobutyl KetoneHCID 8471TriethylamineHCID 68509CumylamineHCID 134936832-Bromo-3,3-dimethylbutanoyl bromide

生成物 1

HCID 53079Bromobutide収率 78.8%

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 (33.8 g) and triethylamine (27.8 g), and α-bromo-tert-butylacetylbromide (64.5 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-tert-butylacetamide (61.5 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-2d3e96851f0e416090d23252d079376e
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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