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Sodium Hydroxide → (2R)-1-[3,5-bis(trifluoromethyl)benzoyl]-2-(3,4-dimethylbenzyl)-4-[4-((3S)-3-carboxymorpholino)-2-butynyl]piperazine

HRID 584242
ノート
印刷プレビュー

反応式

HRID 584242 の反応式
[F:1][C:2]([F:46])([F:45])[C:3]1[CH:4]=[C:5]([CH:38]=[C:39]([C:41]([F:44])([F:43])[F:42])[CH:40]=1)[C:6]([N:8]1[CH2:13][CH2:12][N:11]([CH2:14][C:15]#[C:16][CH2:17][N:18]2[CH2:23][CH2:22][O:21][CH2:20][C@H:19]2[C:24]([O:26]CC)=[O:25])[CH2:10][C@H:9]1[CH2:29][C:30]1[CH:35]=[CH:34][C:33]([CH3:36])=[C:32]([CH3:37])[CH:31]=1)=[O:7].[OH-].[Na+]>C(O)C>[F:44][C:41]([F:42])([F:43])[C:39]1[CH:38]=[C:5]([CH:4]=[C:3]([C:2]([F:1])([F:46])[F:45])[CH:40]=1)[C:6]([N:8]1[CH2:13][CH2:12][N:11]([CH2:14][C:15]#[C:16][CH2:17][N:18]2[CH2:23][CH2:22][O:21][CH2:20][C@H:19]2[C:24]([OH:26])=[O:25])[CH2:10][C@H:9]1[CH2:29][C:30]1[CH:35]=[CH:34][C:33]([CH3:36])=[C:32]([CH3:37])[CH:31]=1)=[O:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 57253530HCID 57253530、化合物

生成物 1

HCID 86588523(2R)-1-[3,5-bis(trifluoromethyl)benzoyl]-2-(3,4-dimethylbenzyl)-4-[4-((3S)-3-carboxymorpholino)-2-butynyl]piperazine収率 64.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of (2R)-1-[3,5-bis(trifluoromethyl)benzoyl]-2-(3,4-dimethylbenzyl)-4-[4-((3S)-3-ethoxycarbonylmorpholino)-2-butynyl]piperazine (0.42 g) in ethanol (30 ml) was added 1N sodium hydroxide solution (30 ml) and the whole was stirred at room temperature for 2 hours. The solvent was removed under reduced pressure and the residual aqueous solution was neutralized with conc. hydrochloric acid. The solution was extracted with dichloromethane. The extract was dried over magnesium sulfate and evaporated in vacuo to give (2R)-1-[3,5-bis(trifluoromethyl)benzoyl]-2-(3,4-dimethylbenzyl)-4-[4-((3S)-3-carboxymorpholino)-2-butynyl]piperazine (0.26 g) as an oil.

後処理

  1. customThe solvent was removed under reduced pressure
  2. extractionThe solution was extracted with dichloromethane
  3. dry with materialThe extract was dried over magnesium sulfate
  4. customevaporated in vacuo

出典と根拠

ORDレコード
ord-3c608db9e8ca4184892a959971f9703b
出典データセット
uspto-grants-2005_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06924278B2

反応ノート

読み込み中…

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