反应 #674305

ord-5e14e4a929f846929471cfb5ccb6d7da

反应方程式

NC(=O)C1CCC(OCc2ccccc2)CC1
4-(benzyloxy)cyclohexanecarboxamide
O=C(OC(=O)C(F)(F)F)C(F)(F)F
trifluoroacetic anhydride
O
H2O
N#CC1CCC(OCc2ccccc2)CC1
4-(benzyloxy)cyclohexanecarbonitrile
收率 97.5%

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    浓缩concentrated
  2. 2
    其他to give the residue
  3. 3
    萃取The aqueous phase was extracted with MTBE (3×50 mL)
  4. 4
    洗涤The combined organic solution was washed with brine (50 mL)
  5. 5
    干燥dried over anhydrous Na2SO4
  6. 6
    浓缩concentrated

实验过程

To a suspension of 4-(benzyloxy)cyclohexanecarboxamide (2.33 g, 10 mmol, 1.0 equiv) in THF (dry, 50 mL) was added trifluoroacetic anhydride (4.16 mL, 30 mmol, 3.0 equiv) dropwise at room temperature. The resulting clear solution was stirred at room temperature for 30 min and then concentrated to give the residue. H2O (50 mL) was added. The aqueous phase was extracted with MTBE (3×50 mL). The combined organic solution was washed with brine (50 mL), dried over anhydrous Na2SO4, concentrated to give 2.1 g (yield 97%) of 4-(benzyloxy)cyclohexanecarbonitrile as a pale yellow oil.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09226923B2uspto-grants-2016_01