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Ethyl chloroacetate → HCID 55288043, 화합물

HRID 2366348
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HRID 2366348 반응식
[H-].[Na+].[NH2:3][C@@H:4]([CH:7]([CH3:9])[CH3:8])[CH2:5][OH:6].Cl[CH2:11][C:12](OCC)=[O:13]>C1(C)C=CC=CC=1>[CH:7]([C@@H:4]1[NH:3][C:12](=[O:13])[CH2:11][O:6][CH2:5]1)([CH3:9])[CH3:8]
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참가 물질

5

반응물 3

HCID 7751Ethyl chloroacetateHCID 24758Sodium hydrideHCID 640993L-Valinol

생성물 1

HCID 55288043HCID 55288043, 화합물수율 67.2%

시약·촉매·용매 1

HCID 1140Toluene용매3회

실험 절차

To an ice-cold, stirred suspension of sodium hydride (2.59 g, 64.8 mmol) in toluene (90 mL) was added dropwise a solution of (S)-2-amino-3-methylbutan-1-ol (3 g, 29.1 mmol) in toluene (60 mL). The reaction was then warmed to room temperature and a solution of ethyl chloroacetate (3.56 g, 29.1 mmol) in toluene (16 mL) was added dropwise. The resulting mixture was heated to reflux for 20 h under nitrogen and then concentrated under vacuum. The residue was purified by flash chromatography to afford 2.8 g of product (MS: (M+H)=144.3).

후처리

  1. temperatureThe resulting mixture was heated
  2. temperatureto reflux for 20 h under nitrogen
  3. concentrationconcentrated under vacuum
  4. customThe residue was purified by flash chromatography

출처 및 근거

ORD 기록
ord-470b20a384fb445c88e5363b5a6f05e1
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08697739B2

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