Nefazodone → Nefazodone hydrochloride

HRID 1636233

反応式

HRID 1636233 の反応式
[CH3:1][CH2:2][C:3]1[N:8]([CH2:9][CH2:10][O:11][C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)[C:6](=[O:7])[N:5]([CH2:18][CH2:19][CH2:20][N:21]2[CH2:26][CH2:25][N:24]([C:27]3[CH:28]=[CH:29][CH:30]=[C:31]([Cl:33])[CH:32]=3)[CH2:23][CH2:22]2)[N:4]=1.[OH-].[Na+]>O>[CH3:1][CH2:2][C:3]1[N:8]([CH2:9][CH2:10][O:11][C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)[C:6](=[O:7])[N:5]([CH2:18][CH2:19][CH2:20][N:21]2[CH2:26][CH2:25][N:24]([C:27]3[CH:28]=[CH:29][CH:30]=[C:31]([Cl:33])[CH:32]=3)[CH2:23][CH2:22]2)[N:4]=1.[ClH:33]

参加物

4

反応物 2

HCID 4449NefazodoneHCID 14798Sodium Hydroxide

生成物 1

HCID 54911Nefazodone hydrochloride

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
42.5 °C

実験手順

Nefazodone HCl was prepared in accordance with Example 2 of U.S. Pat. No. 4,338,317. Nefazodone HCI was dissolved in water with gentle heating (40-45° C.). An equimolar quantity of sodium hydroxide solution (0.1 N) was added with constant stirring while cooling with ice. Nefazodone base precipitated as a sticky gum which was separated and washed repeatedly with water. The base was washed with water until no chloride ions (AgNO3 test) were detected in the washings. Nefazodone base was then dissolved and crystallized from isopropyl alcohol (IPA) to give a solid melting 81-83° C.

後処理

  1. temperaturewhile cooling with ice
  2. customNefazodone base precipitated as a sticky gum which
  3. customwas separated
  4. washwashed repeatedly with water
  5. washThe base was washed with water until no chloride ions (AgNO3 test)
  6. dissolutionNefazodone base was then dissolved
  7. customcrystallized from isopropyl alcohol (IPA)
  8. customto give a solid
  9. custommelting 81-83° C.

出典と根拠

ORDレコード
ord-02174f92564844058b99dde18f2e5844
出典データセット
uspto-grants-2000_03
特許番号
US06034085

関連ノート

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