Triethylamine → Ethyl 3-{[(benzyloxy)carbonyl]amino}propanoate

HRID 17426

반응식

HRID 17426 반응식
Cl.[NH2:2][CH2:3][CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6].Cl[C:11]([O:13][CH2:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)=[O:12].C(N(CC)CC)C>ClCCl>[CH2:14]([O:13][C:11]([NH:2][CH2:3][CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6])=[O:12])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 10387Benzyl chloroformateHCID 458475beta-Alanine, ethyl ester, hydrochloride

생성물 1

HCID 12116647Ethyl 3-{[(benzyloxy)carbonyl]amino}propanoate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Ethyl 3-aminopropionate hydrochloride (2.00 g, 13.0 mmol) was dissolved in dichloromethane (40 ml), and benzyl chloroformate (2.00 ml, 14.1 mmol) was added. With cooling with ice, triethylamine (4.00 ml, 28.9 mmol) was added, followed by stirring at room temperature for 15 hours, then the reaction, liquid was concentrated. Ethyl acetate and water were added, the organic layer was collected, and dried over anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure, the resulting residue was purified by silica gel column chromatography (dichloromethane to dichloromethane:methanol=70:1) to obtain a pale yellow oil (3.26 g, quant).

후처리

  1. additionwas added
  2. customthe reaction, liquid
  3. concentrationwas concentrated
  4. additionEthyl acetate and water were added
  5. customthe organic layer was collected
  6. dry with materialdried over anhydrous sodium sulfate
  7. customThe solvent was evaporated away under reduced pressure
  8. customthe resulting residue was purified by silica gel column chromatography (dichloromethane to dichloromethane:methanol=70:1)
  9. customto obtain a pale yellow oil (3.26 g, quant)

출처 및 근거

ORD 기록
ord-264e2d6a7e9b4546809255c18b4318aa
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07737166B2

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