Chloride → HCID 10446654, 화합물

HRID 128777노트

반응식

HRID 128777 반응식
[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:30])[CH2:26][CH2:27][CH2:28][CH3:29].[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:30])[CH2:26][CH2:27][CH2:28][CH3:29]

참가 물질

8

반응물 5

HCID 312ChlorideHCID 8471TriethylamineHCID 14797Potassium HydroxideHCID 61186Valeryl chlorideHCID 118201402-(2-methoxy-1-naphthyl)ethanamine(SALTDATA: HCl)

생성물 1

HCID 10446654HCID 10446654, 화합물수율 46.8%

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

0.59 g (2.93 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 0.61 cm3 (4.37 mmol) of triethylamine dried over potassium hydroxide, is introduced, followed by 0.42 cm3 (3.54 mmol) of valeryl 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, 0.39 g (1.37 mmol) of N-[2-(2-methoxynaphthyl)ethyl]pentanamide (white solid) is obtained, equivalent to a yield after purification of 47%.

후처리

  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

출처 및 근거

ORD 기록
ord-c7e3182bc99b4fd5ad1d087f4993a2fe
출처 데이터셋
uspto-grants-1995_11
특허 번호
US05464872

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