Triethylamine → Methyl 3-((2-(tert-butoxy)-2-oxoethyl)amino)propanoate

HRID 841137

반응식

HRID 841137 반응식
C(N(CC)CC)C.Cl.[CH3:9][O:10][C:11](=[O:15])[CH2:12][CH2:13][NH2:14].Br[CH2:17][C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19]>C(Cl)Cl>[CH3:9][O:10][C:11](=[O:15])[CH2:12][CH2:13][NH:14][CH2:17][C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 79177tert-Butyl bromoacetateHCID 2734767Methyl 3-aminopropanoate hydrochloride

생성물 1

HCID 14845245Methyl 3-((2-(tert-butoxy)-2-oxoethyl)amino)propanoate수율 14%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
0 °C

실험 절차

Triethylamine (7 mL, 50 mmol) was added to a solution of β-alanine methyl ester hydrochloride (5.25 g, 37.5 mmol) in methylene chloride (100 mL). The solution was cooled to 0° C. and t-butyl bromoacetate (4.88 g, 25 mmol) in methylene chloride (100 mL) was then added. The reaction mixture was warmed to room temperature and stirred overnight. The solvent was removed in vacuo and the residue was taken up in ethyl acetate. The ethyl acetate was washed with saturated NaHCO3, brine, dried over MgSO4, filtered and concentrated in vacuo; 0.80 g (14% yield).

후처리

  1. temperatureThe reaction mixture was warmed to room temperature
  2. customThe solvent was removed in vacuo
  3. washThe ethyl acetate was washed with saturated NaHCO3, brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-e51e580066c04d04b3613901de4d82bf
출처 데이터셋
uspto-grants-2002_04
특허 번호
US06369034B1

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