반응 #648787

ord-c0053f7b23424317bf48f9c4cbbc1b16

반응 조건

온도
60°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과the suspension was filtered through kieselguhr
  2. 2
    기타The solvents were removed in a rotary evaporator
  3. 3
    기타the residue was purified by preparative HPLC (mobile phase: acetonitrile/water gradient)

실험 절차

A solution of 1.67 g (3.86 mmol) of the compound from Example 103A in 8 ml of tetrahydrofuran was added dropwise to 13.5 ml (13.5 mmol) of a 1N solution of lithium aluminum hydride in tetrahydrofuran in 16 ml of tetrahydrofuran at RT under argon. The mixture was stirred at 60° C. for 1 h and then water and acetonitrile were added, and the suspension was filtered through kieselguhr. The solvents were removed in a rotary evaporator, and the residue was purified by preparative HPLC (mobile phase: acetonitrile/water gradient). 1.39 g (92% of theory) of the title compound were obtained.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08063234B2uspto-grants-2011_11