反応式
[F:1][CH:2]([F:15])[O:3][C:4]1[CH:5]=[C:6]2[C:10](=[CH:11][CH:12]=1)[N:9]([CH3:13])[N:8]=[C:7]2I.[CH:16]([Mg]Cl)(C)C.[CH2:21]([Sn:25]([CH2:30][CH2:31][CH2:32][CH3:33])(Cl)[CH2:26][CH2:27][CH3:28])[CH2:22][CH2:23][CH3:24]>C1COCC1>[F:1][CH:2]([F:15])[O:3][C:4]1[CH:5]=[C:6]2[C:10](=[CH:11][CH:12]=1)[N:9]([CH3:13])[N:8]=[C:7]2[Sn:25]([CH2:30][CH2:31][CH2:32][CH3:33])([CH2:26][CH2:27][CH2:28][CH3:16])[CH2:21][CH2:22][CH2:23][CH3:24]参加物
5
実験手順
To a solution of 5-(difluoromethoxy)-3-iodo-1-methyl-1H-indazole (400 mg, 1.23 mmol) in dry THF (15 mL) was added isopropylmagnesium chloride (0.75 mL, 1.3 mmol, 2M in THF) drop-wise at −16° C. under nitrogen atmosphere, stirred for 30 minutes, then dibutylchloro(propyl)stannane (0.5 mL, 1.45 mmol) was added drop-wise, the reaction mixture was warmed to room temperature slowly and stirred for 2 hours. The reaction mixture was quenched with a saturated solution of NH4Cl (40 mL) and extracted with EtOAc (3×30 mL). The combined organic layers were dried over Na2SO4, filtered and concentrated under reduced pressure and the residue was used into the next step without purification (500 mg, crude) as oil.
後処理
- stirringstirred for 2 hours
- customThe reaction mixture was quenched with a saturated solution of NH4Cl (40 mL)
- extractionextracted with EtOAc (3×30 mL)
- dry with materialThe combined organic layers were dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customthe residue was used into the next step without purification (500 mg, crude) as oil
出典と根拠
- ORDレコード
- ord-e3d12928dbe341bb81bba19fe3bc89ef
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08658646B2
関連ノート
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