1,2-Dichloroethane → 5-(2-Cyano-4-trifluoromethylphenoxy)-2-nitrobenzoic acid

HRID 868395ノート

反応式

HRID 868395 の反応式
[C:1]([C:3]1[CH:18]=[C:17]([C:19]([F:22])([F:21])[F:20])[CH:16]=[CH:15][C:4]=1[O:5][C:6]1[CH:7]=[C:8]([CH:12]=[CH:13][CH:14]=1)[C:9]([OH:11])=[O:10])#[N:2].ClCCCl.S(=O)(=O)(O)O.[N+:32]([O-])([O-:34])=[O:33].[K+]>O>[C:1]([C:3]1[CH:18]=[C:17]([C:19]([F:20])([F:21])[F:22])[CH:16]=[CH:15][C:4]=1[O:5][C:6]1[CH:14]=[CH:13][C:12]([N+:32]([O-:34])=[O:33])=[C:8]([CH:7]=1)[C:9]([OH:11])=[O:10])#[N:2]

参加物

6

反応物 4

HCID 111,2-DichloroethaneHCID 1118Sulfuric AcidHCID 24434Potassium NitrateHCID 130136843-(2-Cyano-4-trifluoromethylphenoxy)benzoic acid

生成物 1

HCID 130136855-(2-Cyano-4-trifluoromethylphenoxy)-2-nitrobenzoic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
0 °C

実験手順

The product from (a) (9.22 g) was added in portions to a mixture of 1,2-dichloroethane (25 ml) and concentrated sulphuric acid (40 ml) stirred at 0° C. Potassium nitrate (3.13 g) was then added in portions with stirring at 0° C., over a period of 15 minutes. The mixture was then stirred at 0° C. for 30 minutes, allowed to warm to room temperature, and poured into 200 ml of ice and water. The mixture was stirred until the ice had melted, and filtered with suction. The solid which separated on evaporation of the dichloroethane was washed with water and taken up in ether. The ether solution was treated with charcoal, dried and petroleum (b.p. 40°-60° C.) added. The solid which separated was identified as the required benzoic acid derivative (7.8 g) having a melting point of 190°-192° C.

後処理

  1. stirringwith stirring at 0° C., over a period of 15 minutes
  2. stirringThe mixture was then stirred at 0° C. for 30 minutes
  3. temperatureto warm to room temperature
  4. filtrationfiltered with suction
  5. customThe solid which separated on evaporation of the dichloroethane
  6. washwas washed with water
  7. additionThe ether solution was treated with charcoal
  8. customdried
  9. additionpetroleum (b.p. 40°-60° C.) added
  10. customThe solid which separated

出典と根拠

ORDレコード
ord-ce92ff3eb5bf4641bab5c18f8a3f029d
出典データセット
uspto-grants-1988_10
特許番号
US04778914

反応ノート

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