Nitric Acid → Methyl 4-bromo-5-nitrothiophene-2-carboxylate

HRID 723075

反応式

HRID 723075 の反応式
[N+:1]([O-:4])(O)=[O:2].[CH3:5][O:6][C:7]([C:9]1[S:10][CH:11]=[C:12]([Br:14])[CH:13]=1)=[O:8]>OS(O)(=O)=O>[CH3:5][O:6][C:7]([C:9]1[S:10][C:11]([N+:1]([O-:4])=[O:2])=[C:12]([Br:14])[CH:13]=1)=[O:8]

参加物

4

反応物 2

HCID 944Nitric AcidHCID 12752071Methyl 4-bromothiophene-2-carboxylate

生成物 1

HCID 13291027Methyl 4-bromo-5-nitrothiophene-2-carboxylate

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒2 回

実験手順

The nitrating mixture (HNO3 d=1.42, 2 mL; concentrated H2SO4, 6 mL) was slowly added with stirring, at −5° to −10° C., to 4-Bromothiophene-2-carboxylic acid methyl ester (3 g, 13.57 mmol) dissolved in concentrated H2SO4 (10 mL). After being kept at −5 to −10° C. for 30 min. the mixture was poured over crushed ice. The solid precipitate was separated by filtration and washed with water and dried over P2O5 to give 3.7 g of 4-bromo-5-nitrothiophene-2-carboxylic acid methyl ester as a tan solid, which was used in the next step without further purification.

後処理

  1. additionthe mixture was poured
  2. customover crushed ice
  3. customThe solid precipitate was separated by filtration
  4. washwashed with water
  5. dry with materialdried over P2O5

出典と根拠

ORDレコード
ord-9f2b676568ce42089fc02dfa248c3f0b
出典データセット
uspto-grants-2006_11
特許番号
US07138530B2

関連ノート

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