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

HRID 723075

반응식

HRID 723075 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9f2b676568ce42089fc02dfa248c3f0b
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07138530B2

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