Nitric Acid → HCID 19737188、化合物

HRID 258258ノート

反応式

HRID 258258 の反応式
[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

参加物

4

反応物 2

HCID 944Nitric AcidHCID 19737207HCID 19737207、化合物

生成物 1

HCID 19737188HCID 19737188、化合物収率 63%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-c6be27b2517f4588ab22ee19158d1701
出典データセット
uspto-grants-1993_11
特許番号
US05266556

反応ノート

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