反応 #303162

ord-ea0fa1e3490d4219a94332c92fa087fa

試薬

なし

溶媒

反応条件

温度
55°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度heated to dissolution
  2. 2
    workup.DISTILLATIONThe resulting suspension is distilled at below 80° C.
  3. 3
    温度cooled to below 10° C
  4. 4
    その他The solid is collected
  5. 5
    その他dried

実験手順

Granisetron (60.0 g) and toluene (12 parts) are charged to a suitable reactor and heated to dissolution. Conc. hydrochloric acid (1.1 eq) is added drop wise while maintaining the temperature at 50 to 60° C. The resulting suspension is distilled at below 80° C. to ⅔ volume and cooled to below 10° C. The solid is collected and dried to provide granisetron hydrochloride (53.6-67 g).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08193217B2uspto-grants-2012_06