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Hydrochloric Acid → 4-Bromo-5-methoxy-2-methylaniline

HRID 536339
ノート
印刷プレビュー

反応式

HRID 536339 の反応式
[Br:1][C:2]1[C:7]([O:8][CH3:9])=[CH:6][C:5]([NH:10]C(=O)C)=[C:4]([CH3:14])[CH:3]=1.Cl.[OH-].[Na+]>CO>[Br:1][C:2]1[C:7]([O:8][CH3:9])=[CH:6][C:5]([NH2:10])=[C:4]([CH3:14])[CH:3]=1
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 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 44512476HCID 44512476、化合物

生成物 1

HCID 152785924-Bromo-5-methoxy-2-methylaniline

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
95 °C

実験手順

N-(4-bromo-5-methoxy-2-methylphenyl)acetamide was dissolved in methanol (15 mL) and concentrated HCl (30 mL). The mixture was refluxed at 95° C. overnight. After cooling to room temperature, the mixture was poured into ice water, and basified to pH=12 with conc. NaOH aqueous solution. The mixture was then extracted with ethyl acetate (3×50 mL). The combined organic layer was dried over Na2SO4 and concentrated. The crude product was purified by silica chromatography (15% ethyl acetate in hexanes) to give 4-bromo-5-methoxy-2-methylaniline as a beige solid; 1H NMR (400 mHz, CDCl3) 7.20 (s, 1H), 6.37 (s, 1H), 4.6 (br, 2H), 3.82 (s, 3H), 2.12 (s, 3H).

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

後処理

  1. temperatureAfter cooling to room temperature
  2. extractionThe mixture was then extracted with ethyl acetate (3×50 mL)
  3. dry with materialThe combined organic layer was dried over Na2SO4
  4. concentrationconcentrated
  5. customThe crude product was purified by silica chromatography (15% ethyl acetate in hexanes)

出典と根拠

ORDレコード
ord-997572087dea4e39bea1f5fe0636959a
出典データセット
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08859574B2

反応ノート

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