反応式
[F:1][C:2]1[CH:3]=[N:4][C:5]2[CH:6]=[C:7]([F:18])[C:8](=[O:17])[N:9]3[CH2:13][C:12]([OH:16])([CH2:14][OH:15])[C:11]=1[C:10]=23.C(N(CC)CC)C.[C:26]1([CH3:36])[CH:31]=[CH:30][C:29]([S:32](Cl)(=[O:34])=[O:33])=[CH:28][CH:27]=1>ClCCl.O1CCCC1.C([Sn](=O)CCCC)CCC>[CH3:36][C:26]1[CH:31]=[CH:30][C:29]([S:32]([O:15][CH2:14][C:12]2([OH:16])[C:11]3=[C:2]([F:1])[CH:3]=[N:4][C:5]4[CH:6]=[C:7]([F:18])[C:8](=[O:17])[N:9]([C:10]=43)[CH2:13]2)(=[O:34])=[O:33])=[CH:28][CH:27]=1参加物
7
反応物 3
生成物 1
試薬・触媒・溶媒 3
実験手順
A solution of 3,8-difluoro-4-hydroxy-4-(hydroxymethyl)-4,5-dihydro-7H-pyrrolo[3,2,1-de]-1,5-naphthyridin-7-one (710 mg, 2.79 mmol) in dichloromethane (35 ml) and tetrahydrofuran (35 ml) was treated with triethylamine (0.58 ml, 4.19 mmol), para-toluenesulphonyl chloride (586 mg, 3.07 mmol) and dibutyltin oxide (35 mg, 0.14 mmol). After 6 hours stirring at room temperature under argon, the mixture was evaporated and water (200 ml) was added. The aqueous phase was extracted with dichloromethane (3×200 ml) and the combined organic extracts dried over magnesium sulphate and evaporated to give the desired compound (1.2 g, 100%) which was used without further purification.
後処理
- customthe mixture was evaporated
- additionwater (200 ml) was added
- extractionThe aqueous phase was extracted with dichloromethane (3×200 ml)
- dry with materialthe combined organic extracts dried over magnesium sulphate
- customevaporated
出典と根拠
- ORDレコード
- ord-498ff0b85cae4603b807ffefd9dc6953
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07732460B2
関連ノート
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