反応 #674314

ord-46bdeee1f88d44a59be411178c4965b9

反応方程式

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

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他formed
  2. 2
    抽出The product was extracted with three 100 mL portions of ethyl acetate
  3. 3
    乾燥the combined organic layers dried over sodium sulfate
  4. 4
    ろ過filtered
  5. 5
    濃縮concentrated under reduced pressure at about 40° C.

実験手順

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.

出典

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