Zolpidem → Zolpidem methanesulfonate

HRID 1066185

反応式

HRID 1066185 の反応式
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[N:16]=[C:15]3[N:10]([CH:11]=[C:12]([CH3:17])[CH:13]=[CH:14]3)[C:9]=2[CH2:18][C:19]([N:21]([CH3:23])[CH3:22])=[O:20])=[CH:6][CH:7]=1.[CH3:24][S:25]([OH:28])(=[O:27])=[O:26]>C(O)C>[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:16]=[C:15]3[N:10]([CH:11]=[C:12]([CH3:17])[CH:13]=[CH:14]3)[C:9]=2[CH2:18][C:19]([N:21]([CH3:22])[CH3:23])=[O:20])=[CH:4][CH:3]=1.[CH3:24][S:25]([O-:28])(=[O:27])=[O:26]

参加物

4

反応物 2

HCID 5732ZolpidemHCID 6395Methanesulfonic Acid

生成物 1

HCID 18004025Zolpidem methanesulfonate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

One gram of zolpidem free base is dissolved in 10 ml of ethanol at 50° C. Then 0.313 g (a molar equivalent) of methane sulfonic acid is added at this temperature, the mixture is stirred for 5 minutes and evaporated to dryness under reduced pressure. The residue is treated with 10 ml of acetone, the remaining solid is filtered off and washed with 5 ml of acetone and dried in vacuum oven at 40° C. to yield zolpidem methanesulfonate. A representative DSC curve is shown in FIG. 12.

後処理

  1. customevaporated to dryness under reduced pressure
  2. additionThe residue is treated with 10 ml of acetone
  3. filtrationthe remaining solid is filtered off
  4. washwashed with 5 ml of acetone
  5. customdried in vacuum oven at 40° C.

出典と根拠

ORDレコード
ord-7de80f1e39ee48d580eb39c9d7b667d9
出典データセット
uspto-grants-2001_06
特許番号
US06242460B1

関連ノート

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