Lithium Hydroxide → 4-[4-(4-Trifluoromethyl-phenyl)-piperazin-1-yl]-butyric acid lithium salt

HRID 511066ノート

反応式

HRID 511066 の反応式
C([O:3][C:4](=[O:24])[CH2:5][CH2:6][CH2:7][N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:19]=[CH:18][C:17]([C:20]([F:23])([F:22])[F:21])=[CH:16][CH:15]=2)[CH2:10][CH2:9]1)C.[OH-].[Li+:26]>O1CCCC1.O.C(#N)C>[Li+:26].[F:23][C:20]([F:21])([F:22])[C:17]1[CH:18]=[CH:19][C:14]([N:11]2[CH2:12][CH2:13][N:8]([CH2:7][CH2:6][CH2:5][C:4]([O-:24])=[O:3])[CH2:9][CH2:10]2)=[CH:15][CH:16]=1

参加物

6

反応物 2

HCID 3939Lithium HydroxideHCID 585765934-[4-(4-Trifluoromethyl-phenyl)-piperazin-1-yl]-butyric acid ethyl ester

生成物 1

HCID 585760704-[4-(4-Trifluoromethyl-phenyl)-piperazin-1-yl]-butyric acid lithium salt

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6342Acetonitrile溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

4-[4-(4-Trifluoromethyl-phenyl)-piperazin-1-yl]-butyric acid ethyl ester (660 mg; 1.92 mmol, prepared in accordance with Example 2) and lithium hydroxide are dissolved in a mixture of tetrahydrofuran (2.8 mL) and water (1.2 mL). The resulting mixture is irradiated in a mono-mode microwave oven for 30 minutes at 70° C. The mixture is then diluted with acetonitrile (20 mL) and the precipitate formed is filtered and rinsed with acetonitrile (10 mL). The solid obtained is then dried under high vacuum to deliver the desired product (584 mg; 1.81 mmol).

後処理

  1. customThe resulting mixture is irradiated in a mono-mode microwave oven for 30 minutes at 70° C
  2. customthe precipitate formed
  3. filtrationis filtered
  4. washrinsed with acetonitrile (10 mL)
  5. customThe solid obtained
  6. customis then dried under high vacuum

出典と根拠

ORDレコード
ord-ce965d0904984e019d4eeca57770a8e7
出典データセット
uspto-grants-2015_08
特許番号
US09096524B2

反応ノート

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