反应 #355790

ord-6bb288b443014d99a024b0c3c304e320

反应方程式

CC(C)(C)OC(=O)N[C@H](C(=O)N[C@@H]1CCN(Cc2ccccc2)C1)C(C)(C)C
1a
CC(C)(C)OC(=O)N[C@H](C(=O)N[C@@H]1CCN(Cc2ccccc2)C1)C(C)(C)C
[1-(S)-(1-Benzyl-pyrrolidin-3-(R)-ylcarbamoyl)-2,2-dimethyl-propyl]-carbamic acid tert-butyl ester
CC(C)(C)[C@H](N)C(=O)N[C@@H]1CCN(Cc2ccccc2)C1
2a
CC(C)(C)[C@H](N)C(=O)N[C@@H]1CCN(Cc2ccccc2)C1
2-(S)-Amino-N-(1-benzyl-pyrrolidin-3-(R)-yl)-3,3-dimethyl-butyramide

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The solvent was removed by rotary evaporation
  2. 2
    其他the resulting organic residue was carefully partitioned between dichloromethane
  3. 3
    萃取The organic extract
  4. 4
    干燥was dried over anhydrous sodium sufate
  5. 5
    过滤filtered
  6. 6
    浓缩concentrated

实验过程

A solution of 1a (0.80 g, 2.06 mmole) in 40% trifluoroacetic acid/dichloromethane (15 mL) was stirred at room temperature for 4 h. The solvent was removed by rotary evaporation, and the resulting organic residue was carefully partitioned between dichloromethane and a saturated solution of sodium bicarbonate (30 mL each). The organic extract was dried over anhydrous sodium sufate, filtered, and concentrated to give 2a as a light brown oil. This amine was used without further purification.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07446115B2uspto-grants-2008_11