3-(1-(2,4-bis(trifluoromethyl)phenyl)phthalazin-6-yl)-N-cyclopropyl-4-methylbenzamide → HCID 68452832、化合物

HRID 2357669ノート

反応式

HRID 2357669 の反応式
F[C:2](F)(F)[C:3]1[CH:8]=[C:7](C(F)(F)F)[CH:6]=[CH:5][C:4]=1[C:13]1[C:22]2[C:17](=[CH:18][C:19]([C:23]3[CH:24]=[C:25]([CH:32]=[CH:33][C:34]=3[CH3:35])[C:26]([NH:28]C3CC3)=[O:27])=[CH:20][CH:21]=2)[CH:16]=[N:15][N:14]=1.O[O:39][S:40]([O-:42])=O.[K+].[CH3:44]O.O>>[CH3:35][C:34]1[CH:33]=[CH:32][C:25]([C:26]([NH2:28])=[O:27])=[CH:24][C:23]=1[C:19]1[CH:18]=[C:17]2[C:22](=[CH:21][CH:20]=1)[C:13]([C:4]1[CH:5]=[CH:6][C:7]([S:40]([CH3:44])(=[O:42])=[O:39])=[CH:8][C:3]=1[CH3:2])=[N:14][N:15]=[CH:16]2

参加物

4

反応物 3

HCID 118489893-(1-(2,4-bis(trifluoromethyl)phenyl)phthalazin-6-yl)-N-cyclopropyl-4-methylbenzamideHCID 22242641Methanol--water (1/1)HCID 23707502Potassium hydroxy sulfite

生成物 1

HCID 68452832HCID 68452832、化合物

反応条件

温度
0 °C

実験手順

A solution of 4-methyl-3-(1-(2-methyl-4-(methylthio)phenyl)phthalazin-6-yl)benzamide (170 mg, 0.43 mmol, Method D) in 2 mL of 10/1 methanol/H2O at 0° C. was treated with oxone (262 mg, 0.43 mmol). The mixture stirred at 0° C. for 1 h and then warmed up to RT for 1 h. The reaction was quenched with 20 mL sodium sulfite (sat.) and extracted with 10% MeOH in dichloromethane. The combined organic layers were dried over anhydrous sodium sulfate, filtered and concentrated. The crude material was purified by HPLC to give 4-methyl-3-(1-(2-methyl-4-(methylsulfonyl)phenyl)phthalazin-6-yl)benzamide as a white solid. Found MS (ES+)=432.1 (M+H+).

後処理

  1. temperaturewarmed up to RT for 1 h
  2. customThe reaction was quenched with 20 mL sodium sulfite (sat.)
  3. extractionextracted with 10% MeOH in dichloromethane
  4. dry with materialThe combined organic layers were dried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe crude material was purified by HPLC

出典と根拠

ORDレコード
ord-245186e08d0c4d5e9a7850c4c6c7bdd7
出典データセット
uspto-grants-2010_07
特許番号
US07759337B2

反応ノート

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