反応式
[CH:1]1([C:4]2[O:5][C:6]3[C:7](=[C:9]([C:17]#[N:18])[C:10]([CH3:16])=[C:11]([CH:14]=[O:15])[C:12]=3[F:13])[N:8]=2)[CH2:3][CH2:2]1.O.O.P([O-])(O)(O)=[O:22].[Na+].CC(=CC)C.Cl([O-])=O.[Na+].Cl>C(O)(C)(C)C.O.O1CCCC1.C(OCC)(=O)C>[C:17]([C:9]1[C:7]2[N:8]=[C:4]([CH:1]3[CH2:2][CH2:3]3)[O:5][C:6]=2[C:12]([F:13])=[C:11]([C:14]([OH:22])=[O:15])[C:10]=1[CH3:16])#[N:18]参加物
反応物 5
生成物 1
試薬・触媒・溶媒 4
実験手順
2-Cyclopropyl-7-fluoro-6-formyl-5-methyl-1,3-benzoxazole-4-carbonitrile (I-182) (160 mg, 0.66 mmol) was dissolved in tert-butanol (4.5 ml)-water (3 ml)-tetrahydrofuran (3 ml), then at 0° C., sodium dihydrogenphosphate dihydrate (153 mg, 0.98 mmol), 2-methyl-2-butene (292 μl, 2.62 mmol), sodium chlorite (purity 80%, 222 mg, 1.97 mmol) were added. This was stirred for 15 hours with gradually warming up to room temperature. At 0° C., aqueous 1 N hydrochloric acid solution and ethyl acetate were added to the reaction liquid, followed by stirring at the same temperature for 10 minutes. The aqueous layer was separated, and extracted twice with ethyl acetate. The organic layers were combined, washed with saturated brine, and dried over anhydrous sodium sulfate. The insoluble matter was separated by filtration, the solvent was evaporated away to obtain the entitled compound. This was used in the next reaction as such.
後処理
- stirringby stirring at the same temperature for 10 minutes
- customThe aqueous layer was separated
- extractionextracted twice with ethyl acetate
- washwashed with saturated brine
- dry with materialdried over anhydrous sodium sulfate
- customThe insoluble matter was separated by filtration
- customthe solvent was evaporated away
- customto obtain the entitled compound
- customThis was used in the next reaction as such
出典と根拠
- ORDレコード
- ord-a0ac29dabbb840a9bd73081a2eac2471
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07737166B2
関連ノート
読み込み中…