反应 #674314

ord-46bdeee1f88d44a59be411178c4965b9

反应方程式

COC(=O)C(c1ccccc1)C1CCCCN1.Cl
methylphenidate hydrochloride
[NH4+].[OH-]
ammonium hydroxide
COC(=O)C(c1ccccc1)C1CCCCN1
oil
收率 95.0%
COC(=O)C(c1ccccc1)C1CCCCN1
Methylphenidate
收率 95.0%

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他formed
  2. 2
    萃取The product was extracted with three 100 mL portions of ethyl acetate
  3. 3
    干燥the combined organic layers dried over sodium sulfate
  4. 4
    过滤filtered
  5. 5
    浓缩concentrated under reduced pressure at about 40° C.

实验过程

To a 200 mL beaker was charged 10.0 g (37.1 mmol) racemic-methylphenidate hydrochloride and 135 mL water. About 3.39 g (96.8 mmol) ammonium hydroxide was then added to bring the pH to approximately 9 upon which an oily semi-solid formed. The product was extracted with three 100 mL portions of ethyl acetate, the combined organic layers dried over sodium sulfate, filtered and concentrated under reduced pressure at about 40° C. to provide 8.2 g of a clear, colorless viscous oil (95% yield). The IR spectrum of the oil was consistent with the intended product.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09226925B1uspto-grants-2016_01