Phosphoric Acid → 2-Bromo-N,N-dibutylacetamide

HRID 1275982ノート

反応式

HRID 1275982 の反応式
[Br:1][CH2:2][C:3](Br)=[O:4].[CH2:6]([NH:10][CH2:11][CH2:12][CH2:13][CH3:14])[CH2:7][CH2:8][CH3:9].OP(O)(O)=O>C1(C)C=CC=CC=1>[CH2:6]([N:10]([CH2:11][CH2:12][CH2:13][CH3:14])[C:3](=[O:4])[CH2:2][Br:1])[CH2:7][CH2:8][CH3:9]

参加物

5

反応物 3

HCID 1004Phosphoric Acid2 回HCID 8148DibutylamineHCID 61147Bromoacetyl bromide

生成物 1

HCID 30161612-Bromo-N,N-dibutylacetamide

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

反応条件

温度
0 °C

実験手順

To a solution of bromoacetyl bromide (72.3 mL, 830 mmol) in toluene (500 mL) cooled to 0° C. was added a solution of dibutylamine (280.0 mL, 1.66 mol) in toluene (220 mL) via an addition funnel maintaining the reaction temperature below 10° C. Upon completion of the addition, the reaction mixture was stirred at 0° C. for 15 minutes. A solution of 2.5% aqueous H3PO4 (500 mL) was slowly introduced, and the reaction mixture was allowed to warm to room temperature with vigorous stirring. The solution is 2.5% phosphoric acid by weight. The layers were separated and the organic phase washed with water (500 mL) and concentrated to provide the bromoacetamide as a solution in toluene.

後処理

  1. temperaturemaintaining the reaction temperature below 10° C
  2. additionUpon completion of the addition
  3. temperatureto warm to room temperature with vigorous stirring
  4. customThe layers were separated
  5. washthe organic phase washed with water (500 mL)
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-5a0cc3f828624c9e9bfcdffcae9d359a
出典データセット
uspto-grants-2000_12
特許番号
US06162927

反応ノート

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