2-(2-Naphthoxy)ethanol → 2-[[2-(2-Naphthalenyloxy)ethyl]oxy]thiophene

HRID 2225622

반응식

HRID 2225622 반응식
[CH3:1][O:2][C:3]1[S:4][CH:5]=[CH:6][CH:7]=1.[CH:8]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH:11]=[CH:10][C:9]=1[O:18][CH2:19]CO>C1C=CC=CC=1.C1(C)C=CC(S(O)(=O)=O)=CC=1>[CH:8]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH:11]=[CH:10][C:9]=1[O:18][CH2:19][CH2:1][O:2][C:3]1[S:4][CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 2

HCID 71312-(2-Naphthoxy)ethanolHCID 856102-Methoxythiophene

생성물 1

HCID 190044702-[[2-(2-Naphthalenyloxy)ethyl]oxy]thiophene수율 49.6%

시약·촉매·용매 2

HCID 6101p-Toluenesulfonic acid촉매HCID 241Benzene용매

실험 절차

A solution of 2-methoxythiophene (2.28 g) and 2-(2-naphthalenyloxy)ethanol (4.0 g) in benzene (35 mL) containing para-toluenesulfonic acid (0.02 g) was stirred at reflux for 3 days in a flask equipped with a Soxhlet extractor charged with 4 Å molecular sieves. The mixture was cooled, washed with 0.5N sodium hydroxide solution, dried over anhydrous magnesium sulfate (MgSO4) and evaporated. Crystallization of the residual material from ethanol (30 mL) provided 2.68 g of 2-[[2-(2-naphthalenyloxy)ethyl]oxy]thiophene as colorless flakes, mp 129°-130 ° C.

후처리

  1. temperatureat reflux for 3 days in a flask
  2. customequipped with a Soxhlet extractor
  3. additioncharged with 4 Å molecular sieves
  4. temperatureThe mixture was cooled
  5. washwashed with 0.5N sodium hydroxide solution
  6. dry with materialdried over anhydrous magnesium sulfate (MgSO4)
  7. customevaporated
  8. customCrystallization of the residual material from ethanol (30 mL)

출처 및 근거

ORD 기록
ord-77634a073577487782f20506c3ab9fb5
출처 데이터셋
uspto-grants-1994_09
특허 번호
US05344843

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