반응 #7549

ord-9712d4af6010476b93d689a4fc03c3f7

반응 조건

온도
65°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  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
    기타The crystals precipitated
  5. 5
    여과were collected by filtration

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07087594B2uspto-grants-2006_08