Chloride → HCID 9970416、化合物

HRID 1451548ノート

反応式

HRID 1451548 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:29])[CH2:26][CH2:27][CH3:28].[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:29])[CH2:26][CH2:27][CH3:28]

参加物

8

反応物 5

HCID 312ChlorideHCID 8471TriethylamineHCID 8855Butyryl chlorideHCID 14797Potassium HydroxideHCID 118201402-(2-methoxy-1-naphthyl)ethanamine(SALTDATA: HCl)

生成物 1

HCID 9970416HCID 9970416、化合物収率 48%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

0.45 g (2.23 mmol) of 2-(2-methoxy-1-naphthyl)ethylamine, which is solubilized in 20 cm3 of anhydrous dichloromethane, is introduced into a 100-cm3 two-necked flask under an inert atmosphere. The mixture is cooled with an ice bath and stirred, and 0.47 cm3 (3.37 mmol) of triethylamine dried over potassium hydroxide is introduced, followed by 0.28 cm3 (2.69 mmol) of butyryl chloride. 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, 0.29 g (1.07 mmol) of N-[2-(2-methoxynaphthyl)ethyl]butyramide (white solid) is obtained, equivalent to a yield after purification of 48%.

後処理

  1. additionis introduced into a 100-cm3 two-necked flask under an inert atmosphere
  2. temperatureThe mixture is cooled with an ice bath
  3. additionis 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-ffd1c0b70f1f4e47a6bd3559a1df2385
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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