Nitric Acid → HCID 14625290、化合物

HRID 1031768ノート

反応式

HRID 1031768 の反応式
[Cl:1][C:2]1[N:3]([C:11]2[CH:16]=[CH:15][C:14]([F:17])=[CH:13][C:12]=2[F:18])[N:4]=[C:5]2[C:10]=1[CH2:9][CH2:8][CH2:7][CH2:6]2.[N+:19]([O-])([OH:21])=[O:20]>S(=O)(=O)(O)O>[Cl:1][C:2]1[N:3]([C:11]2[CH:16]=[C:15]([N+:19]([O-:21])=[O:20])[C:14]([F:17])=[CH:13][C:12]=2[F:18])[N:4]=[C:5]2[C:10]=1[CH2:9][CH2:8][CH2:7][CH2:6]2

参加物

4

反応物 2

HCID 944Nitric AcidHCID 146252893-Chloro-2-(2,4-difluorophenyl)-4,5,6,7-tetrahydro-2H-indazole

生成物 1

HCID 14625290HCID 14625290、化合物収率 89.6%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

A solution of 3-chloro-2-(2,4-difluorophenyl)4,5,6,7-tetrahydro-2H-indazole (217 g) in conc. sulfuric acid (1 kg) was cooled to 5° C., and 99 % nitric acid (67 g) was dropwise added thereto at a temperature below about 10° C., followed by stirring for 3 hours. After completion of the reaction, the reaction mixture was added to ice-water (10 kg), and the precipitated crystals were collected by filtration, washed and dried to give 3-chloro-2-(2,4-difluoro-5-nitrophenyl)-4,5,6,7-tetrahydro-2H-indazole (227 g). m.p., 117° -118 ° C. (decomp.).

後処理

  1. customat a temperature below about 10° C.
  2. customAfter completion of the reaction
  3. filtrationthe precipitated crystals were collected by filtration
  4. washwashed
  5. customdried

出典と根拠

ORDレコード
ord-1e214882c6c34c8ab6ace3ebe7c3f0ff
出典データセット
uspto-grants-1990_09
特許番号
US04954626

反応ノート

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