反応 #1179960

ord-241345e4bece42cea07b96a6b7cd45a3

反応方程式

OC1CN(CCCOCCc2ccc3sccc3c2)C1
1-{3-[2-(1-benzothiophen-5-yl)ethoxy]propyl}-3-azetidinol
O=C(O)[C@H](O)[C@@H](O)C(=O)O
L-tartaric acid
CCO
ethanol
O=C(O)[C@H](O)[C@@H](O)C(=O)O.OC1CN(CCCOCCc2ccc3sccc3c2)C1
1-{3-[2-(1-benzothiophen-5-yl)ethoxy]propyl}-3-azetidinol L-tartrate
収率 91.8%

反応条件

温度
65°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONwere added
  2. 2
    workup.DISSOLUTIONdissolution
  3. 3
    workup.STIRRINGat the same temperature and the resulting mixture was stirred at 20 to 30° C. for 1 hour
  4. 4
    その他The crystals precipitated
  5. 5
    ろ過were collected by filtration

実験手順

In 40 mL of ethyl acetate was dissolved 10.0 g of 1-{3-[2-(1-benzothiophen-5-yl)ethoxy]propyl}-3-azetidinol, and 5.15 g of L-tartaric acid and 40 mL of ethanol were added thereto, after which the resulting mixture was heated at 65° C. to effect dissolution. After the resulting solution was stirred at 50° C. for 20 minutes, 40 mL of ethyl acetate was added dropwise thereto at the same temperature and the resulting mixture was stirred at 20 to 30° C. for 1 hour. The crystals precipitated were collected by filtration to obtain 13.9 g of 1-{3-[2-(1-benzothiophen-5-yl)ethoxy]propyl}-3-azetidinol L-tartrate as colorless crystals.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08129535B2uspto-grants-2012_03