N-bromobutanimide → 7-Bromo-3,6,6-trimethyl-1-pyridin-2-yl-5,7-dihydroindazol-4-one

HRID 2084282

反応式

HRID 2084282 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[N:7]1[C:15]2[CH2:14][C:13]([CH3:17])([CH3:16])[CH2:12][C:11](=[O:18])[C:10]=2[C:9]([CH3:19])=[N:8]1.[Br:20]N1C(=O)CCC1=O>C(Cl)(Cl)Cl>[Br:20][CH:14]1[C:15]2[N:7]([C:2]3[CH:3]=[CH:4][CH:5]=[CH:6][N:1]=3)[N:8]=[C:9]([CH3:19])[C:10]=2[C:11](=[O:18])[CH2:12][C:13]1([CH3:16])[CH3:17]

参加物

4

反応物 2

HCID 67184N-bromobutanimideHCID 41652463,6,6-Trimethyl-1-pyridin-2-yl-5,7-dihydroindazol-4-one

生成物 1

HCID 40739867-Bromo-3,6,6-trimethyl-1-pyridin-2-yl-5,7-dihydroindazol-4-one

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
60 °C

実験手順

A mixture of 1-(2-pyridyl)-3,6,6-trimethyl-4-oxo-4,5,6,7-tetrahydroindazole (0.25 g, 0.98 mmol), prepared as described in example 3, and N-bromosuccinimide (0.180 g, 0.98 mmol) in chloroform (6 ml) was stirred at 60° C. for about 4 hours and then washed with water. The organic phase was dried over sodium sulfate and evaporated to dryness. The residue was chromatographed on silica gel (cyclohexane:ethyl acetate=90:10). The title compound was obtained as a colourless solid (0.28 g, 85%): m.p 160-161° C.

後処理

  1. customprepared
  2. washwashed with water
  3. dry with materialThe organic phase was dried over sodium sulfate
  4. customevaporated to dryness
  5. customThe residue was chromatographed on silica gel (cyclohexane:ethyl acetate=90:10)

出典と根拠

ORDレコード
ord-445e38361a5948df8fe163982b494a9a
出典データセット
uspto-grants-2004_04
特許番号
US06716856B1

関連ノート

読み込み中…