Methylphenidate Hydrochloride → Methylphenidate

HRID 242138

反応式

HRID 242138 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]([CH:5]([CH:12]1[NH:17][CH2:16][CH2:15][CH2:14][CH2:13]1)[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=[O:4]

参加物

4

反応物 2

HCID 9280Methylphenidate HydrochlorideHCID 14923Ammonium Hydroxide

生成物 1

HCID 4158Methylphenidate収率 95%

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. 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.

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 dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure at about 40° C.

出典と根拠

ORDレコード
ord-1abda8bbfd7546549d9a2c336e58e008
出典データセット
uspto-grants-2014_02
特許番号
US08653106B2

関連ノート

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