反応 #7547

ord-dbe896ef33d741a789d2585a245fe8e0

反応方程式

OC1CN(CCCOCCc2ccc3sccc3c2)C1
1-{3-[2-(1-benzothiophen-5-yl)ethoxy]propyl}-3-azetidinol
O=C(O)/C=C\C(=O)O
maleic acid
O=C(O)/C=C\C(=O)O.OC1CN(CCCOCCc2ccc3sccc3c2)C1
1-{3-[2-(1-benzothiophen-5-yl)ethoxy]propyl}-3-azetidinol maleate
収率 88.4%

溶媒

反応条件

温度
5°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONby adding
  2. 2
    workup.DISSOLUTIONdissolution
  3. 3
    温度The reaction mixture was slowly cooled
  4. 4
    その他The crystals precipitated
  5. 5
    ろ過were collected by filtration

実験手順

In 56 mL of acetone was dissolved 8.00 g of 1-{3-[2-(1-benzothiophen-5-yl)ethoxy]propyl}-3-azetidinol, followed by adding thereto 3.19 g of maleic acid, and the resulting mixture was heated at 60° C. to effect dissolution. The reaction mixture was slowly cooled and then stirred at 5° C. for 30 minutes. The crystals precipitated were collected by filtration to obtain 9.89 g of 1-{3-[2-(1-benzothiophen-5-yl)ethoxy]propyl}-3-azetidinol maleate as colorless crystals.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07087594B2uspto-grants-2006_08