Ammonium Chloride → (7-Chloro-1,3-dioxaindan-5-yl)methanol
反応式
[Cl:1][C:2]1[C:7]2[O:8][CH2:9][O:10][C:6]=2[CH:5]=[C:4]([CH:11]=[O:12])[CH:3]=1.[BH4-].[Na+].[NH4+].[Cl-]>C1COCC1>[Cl:1][C:2]1[C:7]2[O:8][CH2:9][O:10][C:6]=2[CH:5]=[C:4]([CH2:11][OH:12])[CH:3]=1参加物
5
実験手順
To a solution of 7-chlorobenzo[d][1,3]dioxole-5-carbaldehyde (6.0 g, 33 mmol) in THF (50 mL) was added NaBH4 (2.5 g, 64 mmol)) in portions at 0° C., The mixture was stirred at this temperature for 30 mm and then poured into aqueous NH4Cl solution. The organic layer was separated, and the aqueous phase was extracted with EtOAc (50 mL×3). The combined extracts were dried over Na2SO4 and evaporated under reduced pressure to afford (7-chlorobenzo[d][1,3]dioxol-5-yl)methanol, which was directly used in the next step.
後処理
- customThe organic layer was separated
- extractionthe aqueous phase was extracted with EtOAc (50 mL×3)
- dry with materialThe combined extracts were dried over Na2SO4
- customevaporated under reduced pressure
出典と根拠
- ORDレコード
- ord-721d231310dc4dd9a0ca9c705dbd586e
- 出典データセット
- uspto-grants-2014_01
- 特許番号
- US08623905B2
反応ノート
読み込み中…