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4-tert-Butylphenol → HCID 20097726、化合物

HRID 1769818
ノート
印刷プレビュー

反応式

HRID 1769818 の反応式
[H-].[Na+].[C:3]([C:7]1[CH:12]=[CH:11][C:10]([OH:13])=[CH:9][CH:8]=1)([CH3:6])([CH3:5])[CH3:4].[H][H].F[C:17]1[CH:31]=[CH:30][C:29]([N+:32]([O-:34])=[O:33])=[CH:28][C:18]=1[C:19]([NH:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)=[O:20]>CN(C)C=O.O>[C:3]([C:7]1[CH:8]=[CH:9][C:10]([O:13][C:17]2[CH:31]=[CH:30][C:29]([N+:32]([O-:34])=[O:33])=[CH:28][C:18]=2[C:19]([NH:21][C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=2)=[O:20])=[CH:11][CH:12]=1)([CH3:6])([CH3:4])[CH3:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 73934-tert-ButylphenolHCID 24758Sodium hydrideHCID 98599812-Fluoro-5-nitro-N-phenylbenzamideHCID 178418361HCID 178418361、化合物

生成物 1

HCID 20097726HCID 20097726、化合物収率 47%

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 6228
Dimethylformamide
溶媒
2 回

実験手順

To 0.18 g (6 mmole) of 80% sodium hydride in 7.5 ml of dry dimethylformamide was slowly added 0.9 g (6 mmole) of 4-t-butylphenol in 2.5 ml of dimethylformamide. After cessation of hydrogen evolution, 1.3 g (5 mmole) of solid 2-fluoro-5-nitrobenzanilide was added and the deep red solution was stirred at room temperature for 5 days. The reaction mixture was diluted with water and extracted with ethyl acetate. The organic layer was washed with IN hydrochloric acid, saturated aqueous sodium bicarbonate solution, dried with magnesium sulphate and the solvent removed to yield the crude product. Recrystallisation from methylene chloride and hexare yielded 0.92 g product (47%) m.p. 138°-140° C.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with IN hydrochloric acid, saturated aqueous sodium bicarbonate solution
  3. dry with materialdried with magnesium sulphate
  4. customthe solvent removed
  5. customto yield the crude product
  6. customRecrystallisation from methylene chloride and hexare

出典と根拠

ORDレコード
ord-a99d0930f4244c39b8beddca70842091
出典データセット
uspto-grants-1995_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05382682

反応ノート

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