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

HRID 17426

反応式

HRID 17426 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-264e2d6a7e9b4546809255c18b4318aa
出典データセット
uspto-grants-2010_06
特許番号
US07737166B2

関連ノート

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