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Sodium Hydroxide → HCID 58817653、化合物

HRID 456561
ノート
印刷プレビュー

反応式

HRID 456561 の反応式
[CH3:1][O:2][C:3]([N:5]1[CH2:10][CH2:9][CH:8]([C:11]2[C:12]3[CH:23]=[CH:22][C:21]([C:24]([F:27])([F:26])[F:25])=[CH:20][C:13]=3[S:14][C:15]=2[C:16]([O:18]C)=[O:17])[CH2:7][CH2:6]1)=[O:4].[OH-].[Na+]>C1COCC1.O>[CH3:1][O:2][C:3]([N:5]1[CH2:6][CH2:7][CH:8]([C:11]2[C:12]3[CH:23]=[CH:22][C:21]([C:24]([F:27])([F:25])[F:26])=[CH:20][C:13]=3[S:14][C:15]=2[C:16]([OH:18])=[O:17])[CH2:9][CH2:10]1)=[O:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 58817546HCID 58817546、化合物

生成物 1

HCID 58817653HCID 58817653、化合物収率 92%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a stirred solution of 4-(2-Methoxycarbonyl-6-trifluoromethyl-benzo[b]thiophen-3-yl)-piperidine-1-carboxylic acid methyl ester (1.1 g, 2.7 mmol) in THF (7.0 mL) was added 1 N NaOH (2.97 mL). The resulting mixture was stirred at room temperature overnight when the mixture was diluted with water (50 mL) and washed with ether (100 mL). The aqueous layer was acidified with the addition of 3 N HCl and the product was extracted with EtOAc (2×150 mL). The combined organic layers were washed with brine (50 mL), dried (MgSO4), filtered and evaporated yielding 960 mg (92%) of the desired product as a white solid.

後処理

  1. washwashed with ether (100 mL)
  2. additionThe aqueous layer was acidified with the addition of 3 N HCl
  3. extractionthe product was extracted with EtOAc (2×150 mL)
  4. washThe combined organic layers were washed with brine (50 mL)
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. customevaporated

出典と根拠

ORDレコード
ord-376591a34ba34fccbc1351e3b9049f52
出典データセット
uspto-grants-2007_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07186724B2

反応ノート

読み込み中…

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