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

HRID 67161노트

반응식

HRID 67161 반응식
[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

참가 물질

3

반응물 2

HCID 944Nitric AcidHCID 13052568HCID 13052568, 화합물

생성물 1

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

반응 조건

온도
4 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-707481f0b73e45cb946d5c2aad8239dd
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04345077

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