Nitric Acid → 4-Chloro-3-nitrophenyl cyclopropyl ketone

HRID 2402348ノート

反応式

HRID 2402348 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([CH:10]2[CH2:12][CH2:11]2)=[O:9])=[CH:4][CH:3]=1.[N+:13]([O-])([OH:15])=[O:14]>>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]([CH:10]2[CH2:11][CH2:12]2)=[O:9])=[CH:6][C:7]=1[N+:13]([O-:15])=[O:14]

参加物

3

反応物 2

HCID 944Nitric AcidHCID 811484-Chlorophenyl cyclopropyl ketone

生成物 1

HCID 12682594-Chloro-3-nitrophenyl cyclopropyl ketone

反応条件

温度
5 °C

実験手順

Under argon and at −10° C., 20 g (110.7 mmol) of (4-chlorophenyl)(cyclopropyl)methanone were added slowly to 60 ml of concentrated nitric acid. The reaction mixture was then slowly warmed to 5° C. and stirred at this temperature for 6 h. Carefully, the reaction solution was then added with stirring to about 100 ml of ice-water. This resulted in the precipitation of a white solid which was filtered off with suction and washed repeatedly with water. The solid obtained in this manner was then dried under high vacuum. This gave 24.3 g (97% of theory) of the desired product.

後処理

  1. additionCarefully, the reaction solution was then added
  2. customThis resulted in the precipitation of a white solid which
  3. filtrationwas filtered off with suction
  4. washwashed repeatedly with water
  5. customThe solid obtained in this manner
  6. customwas then dried under high vacuum

出典と根拠

ORDレコード
ord-aff21bc8cc554f5f945f66d09358ccf5
出典データセット
uspto-grants-2014_08
特許番号
US08796335B2

反応ノート

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