Water → N-benzyl-N-(2-chloroethyl)propan-2-amine

HRID 868575

반응식

HRID 868575 반응식
[CH2:1]([N:8]([CH:13]([CH3:15])[CH3:14])[C:9](=O)[CH2:10][Cl:11])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O>C(OCC)C>[CH:13]([N:8]([CH2:1][C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1)[CH2:9][CH2:10][Cl:11])([CH3:15])[CH3:14]

참가 물질

5

반응물 3

HCID 962WaterHCID 2384365N-Benzyl-2-chloro-N-isopropyl-acetamideHCID 21226445Aluminium lithium hydride

생성물 1

HCID 48358N-benzyl-N-(2-chloroethyl)propan-2-amine수율 50.2%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

A solution of 7.66 g of the N-benzyl-2-chloro-N-isopropylacetamide in 20 ml of dry diethyl ether was added dropwise to a suspension of 1.29 g of lithium aluminum hydride in 300 ml of dry diethyl ether with stirring under ice-cooling, and the mixture was heated under reflux for 4 hours. After the reaction mixture was cooled, and to the cooled reaction mixture was added dropwise water with stirring under ice-cooling. Insoluble materials were filtered off. The filtrate was dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified with silica gel column chromatography (eluent: chloroform) to obtain 3.61 g of 2-(N-isopropylbenzylamino)ethyl chloride in an oil.

후처리

  1. temperaturecooling
  2. temperaturethe mixture was heated
  3. temperatureunder reflux for 4 hours
  4. temperatureAfter the reaction mixture was cooled
  5. customto the cooled reaction mixture
  6. stirringwith stirring under ice-
  7. temperaturecooling
  8. filtrationInsoluble materials were filtered off
  9. dry with materialThe filtrate was dried over anhydrous magnesium sulfate
  10. concentrationconcentrated under reduced pressure
  11. customThe residue was purified with silica gel column chromatography (eluent: chloroform)

출처 및 근거

ORD 기록
ord-78754c47888f4305b95fcc2d426f2c38
출처 데이터셋
uspto-grants-1988_10
특허 번호
US04780477

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