反应 #1857562

ord-3325952086a340d2b3fce59dcd131fb9

反应方程式

CCCO[C@H]1CCC[C@H](NC(=O)OC(C)(C)C)C(=O)O[C@@H](C)[C@@H]1CCC(C)C
tert-butyl ((3S,7S,8S,9S)-8-isopentyl-9-methyl-2-oxo-7-propoxyoxonan-3-yl)carbamate
Cl
HCl
C1COCCO1
dioxane
CCCO[C@H]1CCC[C@H]([NH3+])C(=O)O[C@@H](C)[C@@H]1CCC(C)C.[Cl-]
(3S,7S,8S,9S)-8-isopentyl-9-methyl-2-oxo-7-propoxyoxonan-3-aminium chloride

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The solvent was removed under a stream of N2, which
  2. 2
    其他afforded a white solid
  3. 3
    其他This solid was triturated with Et2O (3×3 mL)
  4. 4
    其他the resulting powder was dried under high vacuum for 1 h

实验过程

To a solution of tert-butyl ((3S,7S,8S,9S)-8-isopentyl-9-methyl-2-oxo-7-propoxyoxonan-3-yl)carbamate (330 mg, 0.826 mmol) in DCM (3 mL) was added a solution of HCl in dioxane (2.07 mL, 8.26 mmol, 4M) under N2 and the resulting solution was stirred at room temperature for 2 h. The solvent was removed under a stream of N2, which afforded a white solid. This solid was triturated with Et2O (3×3 mL) and the resulting powder was dried under high vacuum for 1 h to give (3S,7S,8S,9S)-8-isopentyl-9-methyl-2-oxo-7-propoxyoxonan-3-aminium chloride (59): ESIMS m/z 300 ([M+H]+).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09247741B2uspto-grants-2016_02