Nitric Acid → HCID 19737188, 화합물

HRID 258258노트

반응식

HRID 258258 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[C:4]([Cl:12])[C:3]=1[N:13]1[C:21]2[C:16](=[CH:17][CH:18]=[C:19]([C:22]([O:24][CH2:25][CH3:26])=[O:23])[CH:20]=2)[CH:15]=[N:14]1.[N+:27]([O-])([OH:29])=[O:28]>S(=O)(=O)(O)O>[Cl:1][C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[C:4]([Cl:12])[C:3]=1[N:13]1[C:21]2[C:16](=[CH:17][C:18]([N+:27]([O-:29])=[O:28])=[C:19]([C:22]([O:24][CH2:25][CH3:26])=[O:23])[CH:20]=2)[CH:15]=[N:14]1

참가 물질

4

반응물 2

HCID 944Nitric AcidHCID 19737207HCID 19737207, 화합물

생성물 1

HCID 19737188HCID 19737188, 화합물수율 63%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

To a solution of ethyl 1-(2,6-dichloro-4-trifluoromethylphenyl)indazol-6-yl carboxylate [Compound No. 62] (3 g) in conc. sulfuric acid (20 g), fuming nitric acid (0.7 g) was added dropwise while cooling with ice, and the resultant mixture was stirred at room temperature for 3 hours. After completion of the reaction, the reaction mixture was poured into ice water, and the precipitated crystals were collected by filtration, washed and dried. The crystals were purified by silica gel column chromatography with hexane-ethyl acetate (4:1) to give ethyl 1-(2,6-dichloro-4-trifluoromethylphenyl)-5-nitroindazol-6-yl carboxylate (2.1 g).

후처리

  1. temperaturewhile cooling with ice
  2. customAfter completion of the reaction
  3. filtrationthe precipitated crystals were collected by filtration
  4. washwashed
  5. customdried
  6. customThe crystals were purified by silica gel column chromatography with hexane-ethyl acetate (4:1)

출처 및 근거

ORD 기록
ord-c6be27b2517f4588ab22ee19158d1701
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05266556

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