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Ethyl chloroacetate → (R)-5-isopropylmorpholin-3-one

HRID 249932
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HRID 249932 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].[Cl-].[NH4+]>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

6

반응물 4

HCID 7751Ethyl chloroacetateHCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 6950587D-Valinol

생성물 1

HCID 51357136(R)-5-isopropylmorpholin-3-one수율 69.8%

시약·촉매·용매 1

HCID 1140Toluene용매3회

실험 절차

To an ice cold, stirred suspension of sodium hydride (60% in oil, 1.6 g, 40.0 mmol) in toluene (52 mL) was added dropwise a solution of (R)-2-amino-3-methylbutan-1-ol (1.8 g, 17.0 mmol) in toluene (38 mL). After the addition was completed, the reaction mixture was warmed to room temperature and a solution of ethyl chloroacetate (2.3 g, 19.0 mmol) in toluene (8 mL) was added in a dropwise manner. The resulting mixture was then stirred at reflux for 20 h, cooled to room temperature, and solid ammonium chloride (2.1 g, 40.0 mmol) added to the reaction. The mixture was stirred for 20 min and then concentrated under reduced pressure. The crude material was purified by column chromatography (silica gel, 95:5 dichloromethane/methanol) to give (R)-5-isopropylmorpholin-3-one (1.7 g, 68%) as a light yellow solid.

후처리

  1. additionAfter the addition
  2. temperatureat reflux for 20 h
  3. temperaturecooled to room temperature
  4. stirringThe mixture was stirred for 20 min
  5. concentrationconcentrated under reduced pressure
  6. customThe crude material was purified by column chromatography (silica gel, 95:5 dichloromethane/methanol)

출처 및 근거

ORD 기록
ord-1ac3f27640fa4feab989f0cad3520d8e
출처 데이터셋
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07863271B2

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