Donepezil → Donepezil methanesulfonate

HRID 1888018ノート

反応式

HRID 1888018 の反応式
[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[CH3:6][O:7][C:8]1[CH:9]=[C:10]2[CH2:19][CH:18]([CH2:20][CH:21]3[CH2:26][CH2:25][N:24]([CH2:27][C:28]4[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=4)[CH2:23][CH2:22]3)[C:16](=[O:17])[C:11]2=[CH:12][C:13]=1[O:14][CH3:15].C(OCCC)CC>C(O)C>[CH3:6][O:7][C:8]1[CH:9]=[C:10]2[CH2:19][CH:18]([CH2:20][CH:21]3[CH2:22][CH2:23][N:24]([CH2:27][C:28]4[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=4)[CH2:25][CH2:26]3)[C:16](=[O:17])[C:11]2=[CH:12][C:13]=1[O:14][CH3:15].[S:2]([O-:5])(=[O:4])(=[O:3])[CH3:1]

参加物

5

反応物 3

HCID 3152DonepezilHCID 6395Methanesulfonic AcidHCID 8114Propyl ether

生成物 1

HCID 131730793Donepezil methanesulfonate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Methanesulfonic acid (1.3 ml, dissolved in 11 ml of absolute ethanol) is slowly added to a solution of Donepezil (3.79 g) in absolute ethanol (38 ml) with stirring at room temperature, and 50 ml of dipropyl ether is added. The solid precipitated is filtered and dried at 55° C. under vacuum to give the title compound. Melting point: 180.3° C.

後処理

  1. customThe solid precipitated
  2. filtrationis filtered
  3. customdried at 55° C. under vacuum

出典と根拠

ORDレコード
ord-2dc43549994e4f18bcf31875780ac882
出典データセット
uspto-grants-2013_08
特許番号
US08501779B2

反応ノート

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