Benzenesulfinic acid, sodium salt → 5-(1,3-Dioxolan-2-yl)-3-(phenylsulfonyl)-1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-indazole

HRID 1038387ノート

反応式

HRID 1038387 の反応式
[O:1]1[CH2:5][CH2:4][O:3][CH:2]1[C:6]1[CH:7]=[C:8]2[C:12](=[CH:13][CH:14]=1)[N:11]([CH2:15][O:16][CH2:17][CH2:18][Si:19]([CH3:22])([CH3:21])[CH3:20])[N:10]=[C:9]2I.[C:24]1([S:30]([O-:32])=[O:31])[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.[Na+]>>[O:1]1[CH2:5][CH2:4][O:3][CH:2]1[C:6]1[CH:7]=[C:8]2[C:12](=[CH:13][CH:14]=1)[N:11]([CH2:15][O:16][CH2:17][CH2:18][Si:19]([CH3:22])([CH3:21])[CH3:20])[N:10]=[C:9]2[S:30]([C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)(=[O:32])=[O:31]

参加物

3

反応物 2

HCID 2723840Benzenesulfinic acid, sodium saltHCID 584076045-(1,3-Dioxolan-2-yl)-3-iodo-1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-indazole

生成物 1

HCID 584075995-(1,3-Dioxolan-2-yl)-3-(phenylsulfonyl)-1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-indazole

実験手順

The title compound was prepared following the procedure described for Example 9A using 150 mg (0.336 mmol) 5-(1,3-dioxolan-2-yl)-3-iodo-1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-indazole (Example 6A) and 164 mg (1.01 mmol) sodium benzenesulfinate. After cooling, the reaction mixture was filtered, and the filtrate was purified by preparative RP-HPLC (acetonitrile/water+0.05% TFA gradient) to give 55 mg of a product mixture containing the title compound. This mixture was used in the next step without further purification.

後処理

  1. temperatureAfter cooling
  2. filtrationthe reaction mixture was filtered
  3. customthe filtrate was purified by preparative RP-HPLC (acetonitrile/water+0.05% TFA gradient)

出典と根拠

ORDレコード
ord-b55af68931114250a884a301c3b9a3a7
出典データセット
uspto-grants-2013_10
特許番号
US08551989B2

反応ノート

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