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Sodium Hydroxide → HCID 19040962、化合物

HRID 2209729
ノート
印刷プレビュー

反応式

HRID 2209729 の反応式
C([O:4][C:5]1[CH:19]=[C:18]([O:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][O:26][C:27]2[CH:32]=[CH:31][C:30]([C:33]#[N:34])=[CH:29][CH:28]=2)[CH:17]=[CH:16][C:6]=1[C:7]([N:9]([CH:13]([CH3:15])[CH3:14])[CH:10]([CH3:12])[CH3:11])=[O:8])(=O)C.[OH-].[Na+]>C(O)C>[C:33]([C:30]1[CH:29]=[CH:28][C:27]([O:26][CH2:25][CH2:24][CH2:23][CH2:22][CH2:21][O:20][C:18]2[CH:17]=[CH:16][C:6]([C:7]([N:9]([CH:13]([CH3:14])[CH3:15])[CH:10]([CH3:12])[CH3:11])=[O:8])=[C:5]([OH:4])[CH:19]=2)=[CH:32][CH:31]=1)#[N:34]
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 15295289HCID 15295289、化合物

生成物 1

HCID 19040962HCID 19040962、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A stirred solution of 2-acetoxy-4-[5-(4-cyanophenoxy)pentyloxy]-N,N-bis(1-methylethyl)benzamide (10 g, 21.5 mmol) in 250 mL of ethanol is treated with 1N sodium hydroxide solution (25 mL, 25 mmol). After stirring at room temperature for 2 hours, the reaction is concentrated in vacuo. This material is partitioned between ethyl acetate and 1N hydrochloric acid. The organic phase is washed with brine, dried over sodium sulfate, and concentrated in vacuo. The resulting material is purified by chromatography on silica gel (200 g) with 40-50% ethyl acetate/hexane as the eluent to afford 4-[5-(4-cyanophenoxy)pentyloxy]-2-hydroxy-N,N-bis(1-methylethyl)benzamide as a colorless foam.

後処理

  1. concentrationthe reaction is concentrated in vacuo
  2. customThis material is partitioned between ethyl acetate and 1N hydrochloric acid
  3. washThe organic phase is washed with brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe resulting material is purified by chromatography on silica gel (200 g) with 40-50% ethyl acetate/hexane as the eluent

出典と根拠

ORDレコード
ord-1487c1d481424846b81a6c7a1c3dcc87
出典データセット
uspto-grants-1995_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05455274

反応ノート

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