Nitric Acid → N-(5-(6-chloro-3-pyridazinyloxy)-2-nitrophenyl)-1,1,1-trifluoromethanesulfonamide

HRID 67161ノート

反応式

HRID 67161 の反応式
[Cl:1][C:2]1[N:7]=[N:6][C:5]([O:8][C:9]2[CH:10]=[C:11]([NH:15][S:16]([C:19]([F:22])([F:21])[F:20])(=[O:18])=[O:17])[CH:12]=[CH:13][CH:14]=2)=[CH:4][CH:3]=1.[N+:23]([O-])([OH:25])=[O:24]>>[Cl:1][C:2]1[N:7]=[N:6][C:5]([O:8][C:9]2[CH:14]=[CH:13][C:12]([N+:23]([O-:25])=[O:24])=[C:11]([NH:15][S:16]([C:19]([F:20])([F:21])[F:22])(=[O:18])=[O:17])[CH:10]=2)=[CH:4][CH:3]=1

参加物

3

反応物 2

HCID 944Nitric AcidHCID 13052568HCID 13052568、化合物

生成物 1

HCID 20528762N-(5-(6-chloro-3-pyridazinyloxy)-2-nitrophenyl)-1,1,1-trifluoromethanesulfonamide

反応条件

温度
4 °C

実験手順

15 g of 1 was added in portions to 200 ml of chilled (4°-5° C.), stirred 90% nitric acid, and the mixture was stirred at 4° C. for 30 minutes. The resulting mixture was poured into ice water and the resulting solid was filtered. The filter cake was washed with water and purified by silica gel column chromatography, using as eluent a 66:30:4 (v:v:v) mixture of hexane, ethyl acetate and tetrahydrofuran, to give 2, as an amber glassy solid.

後処理

  1. temperatureof chilled (4°-5° C.)
  2. filtrationthe resulting solid was filtered
  3. washThe filter cake was washed with water
  4. custompurified by silica gel column chromatography
  5. additiona 66:30:4 (v:v:v) mixture of hexane, ethyl acetate and tetrahydrofuran
  6. customto give 2

出典と根拠

ORDレコード
ord-707481f0b73e45cb946d5c2aad8239dd
出典データセット
uspto-grants-1982_08
特許番号
US04345077

反応ノート

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