Water → HCID 10263076、化合物

HRID 129034

反応式

HRID 129034 の反応式
C([Li])CCC.[CH:6]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1Br)([CH3:8])[CH3:7].[CH2:16]([N:18]([CH2:22][CH3:23])[C:19](Cl)=[O:20])[CH3:17].O>CCOCC>[CH:6]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[C:19]([N:18]([CH2:22][CH3:23])[CH2:16][CH3:17])=[O:20])([CH3:8])[CH3:7]

参加物

6

反応物 4

HCID 962WaterHCID 6916Diethylcarbamoyl chlorideHCID 23475o-BromocumeneHCID 178418339Butyllithium

生成物 1

HCID 10263076HCID 10263076、化合物収率 80%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

n-Butyllithium (2.5M, 100 mL) was added with stirring under nitrogen at 0°-5° C. during ten minutes to a solution of 2-isopropylbromobenzene in anhydrous ether (500 mL). The mixture was allowed to warm to room temperature, stirred at room temperature for six hours, and cooled to -60° C. A solution of diethylcarbamyl chloride (34 g) in anhydrous ether (50 mL) was added during 20 minutes while maintaining the temperature below -50° C. The temperature was allowed to rise to room temperature during one hour. Water (100 mL) was added. The ether layer was washed with saturated aqueous sodium chloride (200 mL), dried over magnesium sulfate and stripped of ether. Distillation of the residue (80°-90° C./0.1 mm Hg) gave 2-isopropyl-N,N-diethylbenzamide (44 g, 80% yield).

後処理

  1. temperaturecooled to -60° C
  2. temperaturewhile maintaining the temperature below -50° C
  3. waitto rise to room temperature during one hour
  4. washThe ether layer was washed with saturated aqueous sodium chloride (200 mL)
  5. dry with materialdried over magnesium sulfate
  6. distillationDistillation of the residue (80°-90° C./0.1 mm Hg)

出典と根拠

ORDレコード
ord-f791e72d887c4a629510bfe1bcab36b4
出典データセット
uspto-grants-1995_11
特許番号
US05466701

関連ノート

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