Nitric Acid → Methyl 5-nitrothiophene-3-carboxylate

HRID 450030

反応式

HRID 450030 の反応式
[CH3:1][O:2][C:3]([C:5]1[CH:9]=[CH:8][S:7][CH:6]=1)=[O:4].[N+:10]([O-])([OH:12])=[O:11].C(OC(=O)C)(=O)C>C(O)(=O)C>[CH3:1][O:2][C:3]([C:5]1[CH:9]=[C:8]([N+:10]([O-:12])=[O:11])[S:7][CH:6]=1)=[O:4]

参加物

5

反応物 3

HCID 944Nitric AcidHCID 7918Acetic AnhydrideHCID 574151Methyl 3-thiophenecarboxylate

生成物 1

HCID 2740231Methyl 5-nitrothiophene-3-carboxylate収率 42%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

反応条件

温度
40 °C

実験手順

To a solution of 3-thiophene carboxylic acid methyl ester (1.8 g, 12.68 mmol) in acetic acid (7.5 ml) was added a mixture of nitric acid (0.67 ml), acetic acid (7.5 ml) and acetic anhydride (4.3 ml) at 0-10° C. The reaction mixture was stirred at 40° C. for 1 hr and then poured into crushed ice. The solid was filtered, washed with cold water and dried. The compound was recrystallised using ether/hexane to give 5-nitro-thiophene-3-carboxylic acid methyl ester (1.0 g, 42%).

後処理

  1. additionpoured
  2. custominto crushed ice
  3. filtrationThe solid was filtered
  4. washwashed with cold water
  5. customdried
  6. customThe compound was recrystallised

出典と根拠

ORDレコード
ord-5a4e6afa0cb94984b084eedef3055e94
出典データセット
uspto-grants-2013_07
特許番号
US08486962B2

関連ノート

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