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

HRID 894929노트

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HRID 894929 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

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온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-911f047edde345b1851bb80170794e69
출처 데이터셋
uspto-grants-1981_08
특허 번호
US04285723

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