Monoperoxyphthalic Acid Magnesium Salt → 4-{2-[3,4-Bis(difluoromethoxy)phenyl]-2-{6-[4-(trifluoromethoxy)phenoxy]-3-pyridyl}ethyl}pyridine-N-oxide

HRID 567948

反応式

HRID 567948 の反応式
[F:1][CH:2]([F:40])[O:3][C:4]1[CH:5]=[C:6]([CH:14]([C:22]2[CH:23]=[N:24][C:25]([O:28][C:29]3[CH:34]=[CH:33][C:32]([O:35][C:36]([F:39])([F:38])[F:37])=[CH:31][CH:30]=3)=[CH:26][CH:27]=2)[CH2:15][C:16]2[CH:21]=[CH:20][N:19]=[CH:18][CH:17]=2)[CH:7]=[CH:8][C:9]=1[O:10][CH:11]([F:13])[F:12].C1C=C(C([O-])=[O:48])C(C(O[O-])=O)=CC=1.[Mg+2]>C(Cl)Cl.CO>[F:40][CH:2]([F:1])[O:3][C:4]1[CH:5]=[C:6]([CH:14]([C:22]2[CH:23]=[N:24][C:25]([O:28][C:29]3[CH:34]=[CH:33][C:32]([O:35][C:36]([F:39])([F:38])[F:37])=[CH:31][CH:30]=3)=[CH:26][CH:27]=2)[CH2:15][C:16]2[CH:21]=[CH:20][N+:19]([O-:48])=[CH:18][CH:17]=2)[CH:7]=[CH:8][C:9]=1[O:10][CH:11]([F:13])[F:12]

参加物

5

反応物 2

HCID 10130449Monoperoxyphthalic Acid Magnesium Salt2 回HCID 212627884-{2-[3,4-Bis(difluoromethoxy)phenyl]-2-{6-[4-(trifluoromethoxy)phenoxy]-3-pyridyl}ethyl}pyridine

生成物 1

HCID 212628044-{2-[3,4-Bis(difluoromethoxy)phenyl]-2-{6-[4-(trifluoromethoxy)phenoxy]-3-pyridyl}ethyl}pyridine-N-oxide収率 162%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of 4-{2-[3,4-bis(difluoromethoxy)phenyl]-2-{6-[4-(trifluoromethoxy)phenoxy]-3-pyridyl}ethyl}pyridine (340 mg, 0.598 mmol) from Step 5 above in a mixture of 6 mL of CH2Cl2 and 0.6 mL of MeOH, was added MMPP (222 mg, 0.359 mmol) in one portion. The mixture was stirred 24 h at room temperature and the reaction was completed with an other 50 mg of MMPP. The reaction was quenched with a saturated aqueous NaHCO3 solution and diluted with CH2Cl2. The organic layer was washed with brine, dried over MgSO4 and concentrated under reduced pressure. The residue was purified by flash chromatography on silica gel (5% MeOH/CH2Cl2) to afford the title compound as an amorphous solid (340 mg, 97%).

後処理

  1. customThe reaction was quenched with a saturated aqueous NaHCO3 solution
  2. additiondiluted with CH2Cl2
  3. washThe organic layer was washed with brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by flash chromatography on silica gel (5% MeOH/CH2Cl2)

出典と根拠

ORDレコード
ord-ebb6f3d8ed0940de80ad1768c155f568
出典データセット
uspto-grants-2001_01
特許番号
US06180650B2

関連ノート

読み込み中…