Methylphenidate Hydrochloride → Dexmethylphenidate

HRID 587133

反応式

HRID 587133 の反応式
[CH3:1][O:2][C:3]([CH:5]([CH:12]1[NH:17][CH2:16][CH2:15][CH2:14][CH2:13]1)[C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=1)=[O:4].Cl.[OH-].[NH4+]>O>[CH3:1][O:2][C:3]([C@H:5]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)[C@@H:12]1[NH:17][CH2:16][CH2:15][CH2:14][CH2:13]1)=[O:4]

参加物

4

反応物 2

HCID 9280Methylphenidate HydrochlorideHCID 14923Ammonium Hydroxide

生成物 1

HCID 154101Dexmethylphenidate収率 98%

試薬・触媒・溶媒 1

HCID 962Water溶媒

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

後処理

  1. customformed
  2. extractionThe product was extracted with three 100 mL portions of ethyl acetate
  3. dry with materialthe combined organic layers were dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customat 40° C.

出典と根拠

ORDレコード
ord-645bf87f5737445791c0f383d910c826
出典データセット
uspto-grants-2016_01
特許番号
US09226925B1

関連ノート

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