反応 #674315

ord-645bf87f5737445791c0f383d910c826

反応方程式

COC(=O)C(c1ccccc1)C1CCCCN1.Cl
methylphenidate hydrochloride
[NH4+].[OH-]
Ammonium hydroxide
COC(=O)[C@H](c1ccccc1)[C@H]1CCCCN1
oil
収率 98.0%
COC(=O)[C@H](c1ccccc1)[C@H]1CCCCN1
d-Methylphenidate
収率 98.0%

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 were dried over sodium sulfate
  4. 4
    ろ過filtered
  5. 5
    濃縮concentrated
  6. 6
    その他at 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. Ammonium hydroxide (3.40 g; 96.8 mmol) 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 were dried over sodium sulfate, filtered and concentrated under reduce pressure at 40° C. to provide 8.5 g of a clear, colorless viscous oil (98% yield). The free base was characterized by FTIR and found to be consistent with the anticipated structure

出典

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