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Sodium hydride → HCID 19381508、化合物

HRID 2209738
ノート
印刷プレビュー

反応式

HRID 2209738 の反応式
[OH:1][C:2]1[CH:16]=[CH:15][C:5]([C:6]([N:8]([CH:12]([CH3:14])[CH3:13])[CH:9]([CH3:11])[CH3:10])=[O:7])=[CH:4][C:3]=1[O:17][CH3:18].[H-].[Na+].[C:21]([C:23]1[CH:34]=[CH:33][C:26]([O:27][CH2:28][CH2:29][CH2:30][CH2:31]Cl)=[CH:25][CH:24]=1)#[N:22]>CN(C)C=O>[C:21]([C:23]1[CH:34]=[CH:33][C:26]([O:27][CH2:28][CH2:29][CH2:30][CH2:31][O:1][C:2]2[CH:16]=[CH:15][C:5]([C:6]([N:8]([CH:9]([CH3:11])[CH3:10])[CH:12]([CH3:13])[CH3:14])=[O:7])=[CH:4][C:3]=2[O:17][CH3:18])=[CH:25][CH:24]=1)#[N:22]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 19381506HCID 19381506、化合物HCID 217472594-Hydroxy-3-methoxy-N,N-di(propan-2-yl)benzamide

生成物 1

HCID 19381508HCID 19381508、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
0 °C

実験手順

A stirred solution of 4-hydroxy-3-methoxy-N,N-bis(1-methylethyl)benzamide (1.0 g, 4.0 mmol) in 50 mL of N,N-dimethylformamide is treated with 60% sodium hydride (160 mg, 4.0 mmol). After stirring at 0° C. for 10 minutes, the reaction is treated with 4-(4-cyanophenoxy)butyl chloride (835 mg, 4.0 mmol) and stirred at 60° C. for 4 days. The reaction is partitioned between diethyl ether and water. The organic layer is washed with brine, dried over magnesium sulfate, and concentrated in vacuo. The resulting material is purified by chromatography on silica gel (30 g) with 60 % ethyl acetate/hexane as the eluent to afford 4-[4-(4-cyanophenoxy)butoxy]-3-methoxy-N,N-bis(1-methylethyl)benzamide as an oil.

後処理

  1. stirringstirred at 60° C. for 4 days
  2. customThe reaction is partitioned between diethyl ether and water
  3. washThe organic layer is washed with brine
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe resulting material is purified by chromatography on silica gel (30 g) with 60 % ethyl acetate/hexane as the eluent

出典と根拠

ORDレコード
ord-0301d4a6d49f46cdab83449a008b4330
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

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート