HCID 59457726、化合物 → HCID 59457678、化合物
反応式
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([C:8]#[C:9][Si](C)(C)C)[C:3]=1[CH2:14][C:15]([O:17]CC)=[O:16]>[OH-].[Na+].CO>[C:8]([C:4]1[CH:5]=[CH:6][CH:7]=[C:2]([F:1])[C:3]=1[CH2:14][C:15]([OH:17])=[O:16])#[CH:9]参加物
4
実験手順
A stirred solution of 331 (607 mg, 2.18 mmol) and IN NaOH (5.5 mL) in methanol (15 mL) was heated at 45° C. for 16 h under nitrogen. The reaction mixture was allowed to cool to room temperature; it was then concentrated, diluted with water, and washed with hexanes. The aqueous layer was collected, acidified with 3N HCl and extracted twice with AcOEt. The organic extract was dried over anhydrous magnesium sulfate, filtered, and concentrated to afford title compound 332 (400 mg, 94% yield, mono-hydrate) as an orange sticky solid. LCMS: 201.1 (M+Na)+.
後処理
- concentrationit was then concentrated
- additiondiluted with water
- washwashed with hexanes
- customThe aqueous layer was collected
- extractionextracted twice with AcOEt
- extractionThe organic extract
- dry with materialwas dried over anhydrous magnesium sulfate
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-cae76e8cfe544fb4bc83698de2325227
- 出典データセット
- uspto-grants-2010_09
- 特許番号
- US07790729B2
反応ノート
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