Sodium Hydroxide → (+-)-Ethopropazine

HRID 473792ノート

反応式

HRID 473792 の反応式
[CH3:1][CH2:2][N:3]([CH:6]([CH2:8][N:9]1[C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=2[S:16][C:15]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]1=2)[CH3:7])[CH2:4][CH3:5].Cl.[OH-].[Na+]>C(Cl)Cl>[CH3:5][CH2:4][N:3]([CH:6]([CH2:8][N:9]1[C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=2[S:16][C:15]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]1=2)[CH3:7])[CH2:2][CH3:1]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 122824Ethopropazine hydrochloride

生成物 1

HCID 3290(+-)-Ethopropazine収率 20%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

In other studies, racemic ethopropazine hydrochloride salt was mixed with methylene chloride and 2M sodium hydroxide. The resulting suspension was agitated and the organic layer collected. After drying, the solvent was removed by rotary evaporation to give racemic ethopropazine base (4.0 g, 0.013 mol) that reacted with dibenzoyl-D-tartaric acid (4.4 g, 0.012 mol) in acetone with agitation. A white precipitate was collected after a few hours. After two recrystallization steps from absolute ethanol, a 99+% crystal was obtained, which was converted to ethopropazine hydrochloride salt. Yield: 20%. From the mother liquor, another diastereomeric salt was obtained as white precipitate, which was also recrystalized twice from absolute ethanol before converting to hydrochloride salt. Yield: 20%.

後処理

  1. customthe organic layer collected
  2. customAfter drying
  3. customthe solvent was removed by rotary evaporation

出典と根拠

ORDレコード
ord-111753f8838146109fadd9eb5eed9517
出典データセット
uspto-grants-2014_01
特許番号
US08637503B2

反応ノート

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