N-Methylbenzylamine → (Benzyl-methyl-amino)-acetic acid methyl ester

HRID 480241노트

반응식

HRID 480241 반응식
Br[CH2:2][C:3]([O:5][CH3:6])=[O:4].[CH3:7][NH:8][CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.CCN(C(C)C)C(C)C>C(Cl)Cl>[CH3:6][O:5][C:3](=[O:4])[CH2:2][N:8]([CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[CH3:7]

참가 물질

5

반응물 3

HCID 7669N-MethylbenzylamineHCID 60984Methyl bromoacetateHCID 81531Diisopropylethylamine

생성물 1

HCID 11229312(Benzyl-methyl-amino)-acetic acid methyl ester

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

Methyl bromoacetate (10 g, 65.4 mmol, 1.0 equiv) was dissolved in 100 mL of CH2Cl2 which was then cooled to 0° C. N-Methylbenzylamine (7.92 g, 65.4 mmol, 1.0 equiv) was added dropwise over a 10 min period at which time Hunig's base (21 g, 163 mmol, 2.49 equiv) was added and the reaction was allowed to warm to room temperature and was stirred for 16 h. The reaction was diluted with 50 mL of saturated bicarbarbonate and the layers were separated. The organic layer was washed once more with 50 mL of sodium bicarbonate, dried over Na2SO4, decanted and concentrated to a yellow oil which was used in the next step without further purification.

후처리

  1. additionwas added
  2. temperatureto warm to room temperature
  3. additionThe reaction was diluted with 50 mL of saturated bicarbarbonate
  4. customthe layers were separated
  5. washThe organic layer was washed once more with 50 mL of sodium bicarbonate
  6. dry with materialdried over Na2SO4
  7. customdecanted
  8. concentrationconcentrated to a yellow oil which
  9. customwas used in the next step without further purification

출처 및 근거

ORD 기록
ord-80da9c884ca942a2b874fa572c3be14d
출처 데이터셋
uspto-grants-2003_11
특허 번호
US06649642B2

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