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

HRID 2225622ノート

反応式

HRID 2225622 の反応式
[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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6101p-Toluenesulfonic acid触媒HCID 241Benzene溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-77634a073577487782f20506c3ab9fb5
出典データセット
uspto-grants-1994_09
特許番号
US05344843

反応ノート

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