Chloride → HCID 10244203、化合物

HRID 1451547ノート

反応式

HRID 1451547 の反応式
[CH3:1][O:2][C:3]1[CH:12]=[CH:11][C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]=1[CH2:13][CH2:14][NH2:15].C(N(CC)CC)C.[OH-].[K+].[C:25](Cl)(=[O:28])[CH2:26][CH3:27].[Cl-]>ClCCl.O>[CH3:1][O:2][C:3]1[CH:12]=[CH:11][C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]=1[CH2:13][CH2:14][NH:15][C:25](=[O:28])[CH2:26][CH3:27]

参加物

8

反応物 5

HCID 312ChlorideHCID 8471TriethylamineHCID 14797Potassium HydroxideHCID 62324Propionyl chlorideHCID 118201402-(2-methoxy-1-naphthyl)ethanamine(SALTDATA: HCl)

生成物 1

HCID 10244203HCID 10244203、化合物収率 39.1%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

1.40 g (6.96 mmol) of 2-(2-methoxynaphthyl)ethylamine, which is solubilized in 20 cm3 of anhydrous dichloromethane, are introduced into a 100-cm3 two-necked flask under an inert atmosphere. The mixture is cooled with an ice bath and stirred, and 1.5 cm3 (10.4 mmol) of triethylamine dried over potassium hydroxide and 0.7 cm3 (8.056 mmol) of propanoyl chloride are introduced. After the introduction of the reactants, the ice bath is removed and reaction is allowed to proceed at room temperature for 30 min. Hydrolysis of the excess chloride is carried out by pouring the reaction mixture into water. After extraction three times with dichloromethane, the organic phase is dried over magnesium sulfate. After evaporation of the solvent and recrystallization of the solid obtained, in the heated state, in a pentane/ethyl acetate mixture, 0.70 g (2.72 mmol) of N-[2-(2-methoxy-1-naphthyl)ethyl]propionamide (white solid) is obtained, equivalent to a yield after purification of 39%. ##STR19##

後処理

  1. additionare introduced into a 100-cm3 two-necked flask under an inert atmosphere
  2. temperatureThe mixture is cooled with an ice bath
  3. additionare introduced
  4. customAfter the introduction of the reactants, the ice bath is removed
  5. customreaction
  6. extractionAfter extraction three times with dichloromethane
  7. dry with materialthe organic phase is dried over magnesium sulfate
  8. customAfter evaporation of the solvent and recrystallization of the solid
  9. customobtained, in the heated state, in a pentane/ethyl acetate mixture

出典と根拠

ORDレコード
ord-c30a9373490a4a23878cd8fa75d5f716
出典データセット
uspto-grants-1997_02
特許番号
US05604261

反応ノート

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