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

HRID 868575

反応式

HRID 868575 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-78754c47888f4305b95fcc2d426f2c38
出典データセット
uspto-grants-1988_10
特許番号
US04780477

関連ノート

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