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

HRID 1275982노트

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HRID 1275982 반응식
[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]

참가 물질

5

반응물 3

HCID 1004Phosphoric Acid2회HCID 8148DibutylamineHCID 61147Bromoacetyl bromide

생성물 1

HCID 30161612-Bromo-N,N-dibutylacetamide

시약·촉매·용매 1

HCID 1140Toluene용매2회

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온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5a0cc3f828624c9e9bfcdffcae9d359a
출처 데이터셋
uspto-grants-2000_12
특허 번호
US06162927

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