3-(2-fluoro-pyridin-4-yl)-5-nitro-1-trityl-1H-indazole → 3-(2-Methoxy-pyridin-4-yl)-5-nitro-1-trityl-1H-indazole

HRID 1020946ノート

反応式

HRID 1020946 の反応式
[O:1]([CH3:3])[K].CO.C1(C)C=CC=CC=1.F[C:14]1[CH:19]=[C:18]([C:20]2[C:28]3[C:23](=[CH:24][CH:25]=[C:26]([N+:29]([O-:31])=[O:30])[CH:27]=3)[N:22]([C:32]([C:45]3[CH:50]=[CH:49][CH:48]=[CH:47][CH:46]=3)([C:39]3[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=3)[C:33]3[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=3)[N:21]=2)[CH:17]=[CH:16][N:15]=1>>[CH3:3][O:1][C:14]1[CH:19]=[C:18]([C:20]2[C:28]3[C:23](=[CH:24][CH:25]=[C:26]([N+:29]([O-:31])=[O:30])[CH:27]=3)[N:22]([C:32]([C:45]3[CH:50]=[CH:49][CH:48]=[CH:47][CH:46]=3)([C:39]3[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=3)[C:33]3[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=3)[N:21]=2)[CH:17]=[CH:16][N:15]=1

参加物

3

反応物 2

HCID 583719213-(2-fluoro-pyridin-4-yl)-5-nitro-1-trityl-1H-indazoleHCID 178501899HCID 178501899、化合物

生成物 1

HCID 673446273-(2-Methoxy-pyridin-4-yl)-5-nitro-1-trityl-1H-indazole収率 100%

反応条件

温度
70 °C

実験手順

In a 250 ml pressure vessel, 3-(2-Fluoro-pyridin-4-yl)-5-nitro-1-trityl-1H-indazole 3BV (5.005 g, 10.0 mmole) was dissolved in 0.1N KOCH3/MeOH/Toluene (Acros, 150 mL, 15.0 mmole) under dry N2 gas. The pressure vessel was tightly sealed and heated under stirring at 70° C. for 24 hours. The pressure vessel was cooled to 0° C. in ice-bath before opening. The contents of the pressure vessel were transferred to 500 ml RBF and evaporated to dryness. The resulting solid was dissolved in CH2Cl2 and washed with saturated NaCl solution and dried over MgSO4. The solvent was evaporated to dryness and dried under high vacuum to yield 4BV as a brown solid (5.12 g, 100%).

後処理

  1. customThe pressure vessel was tightly sealed
  2. temperatureheated
  3. temperatureThe pressure vessel was cooled to 0° C. in ice-bath
  4. customevaporated to dryness
  5. dissolutionThe resulting solid was dissolved in CH2Cl2
  6. washwashed with saturated NaCl solution
  7. dry with materialdried over MgSO4
  8. customThe solvent was evaporated to dryness
  9. customdried under high vacuum

出典と根拠

ORDレコード
ord-3ec114f409f8495abaa60812f278037e
出典データセット
uspto-grants-2014_05
特許番号
US08716483B2

反応ノート

読み込み中…