Nitric Acid → HCID 56763846、化合物

HRID 605310ノート

反応式

HRID 605310 の反応式
[N+:1]([O-:4])(O)=[O:2].[CH2:5]([O:7][C:8]([C:10]1[S:11][C:12]([Cl:15])=[CH:13][CH:14]=1)=[O:9])[CH3:6]>>[CH2:5]([O:7][C:8]([C:10]1[S:11][C:12]([Cl:15])=[C:13]([N+:1]([O-:4])=[O:2])[CH:14]=1)=[O:9])[CH3:6]

参加物

3

反応物 2

HCID 944Nitric AcidHCID 521808Ethyl 5-chlorothiophene-2-carboxylate

生成物 1

HCID 56763846HCID 56763846、化合物収率 55%

反応条件

温度
10 °C

実験手順

A solution of fuming nitric acid (75 mL) was cooled to 10° C. followed by the addition of 5-chloro-thiophene-2-carboxylic acid ethyl ester (15 g, 78.7 mmol). The resulting mixture was stirred for 30 minutes at 10° C. followed by the addition of ice water. The solution was then extracted with ethyl acetate and dried, then concentrated under vacuum and purified by column chromatography using silica gel to provide 10.29 g (55%) of the title product.

後処理

  1. extractionThe solution was then extracted with ethyl acetate
  2. customdried
  3. concentrationconcentrated under vacuum
  4. custompurified by column chromatography

出典と根拠

ORDレコード
ord-ab80c8d83b084772a16961669b11eb2b
出典データセット
uspto-grants-2011_03
特許番号
US07910595B2

反応ノート

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