Hydrochloric Acid → HCID 30080799、化合物
反応式
[N:1]([CH2:4][C@@H:5]([OH:15])[CH2:6][O:7][C:8]1[CH:13]=[CH:12][C:11]([F:14])=[CH:10][CH:9]=1)=[N+]=[N-].Cl>CC(O)C>[NH2:1][CH2:4][C@@H:5]([OH:15])[CH2:6][O:7][C:8]1[CH:13]=[CH:12][C:11]([F:14])=[CH:10][CH:9]=1参加物
4
反応条件
- 温度
- 80 °C
実験手順
A mixture of (R)-1-azido-3-(4-fluoro-phenoxy)-propan-2-ol (4.83 g, 22.9 mmol) NaBH4 (1.73 g, 45.8 mmol) in iPrOH (100 mL) was stirred at 80° C. for 24 h. After cooling to RT, aq. HCl (200 mL, 0.25 M) was added, washed with CH2Cl2 (100 mL). Saturated aq. K2CO3 (150 mL) was added to the aqueous phase. The product was extracted with CH2Cl2 (2×100 mL), extracts were dried over Na2SO4 and evaporated. The residue was dried under vacuum. White solid, 2.20 g (11.9 mmol, 52%). LCMS [M+H]+ 186.1
後処理
- temperatureAfter cooling to RT
- washwashed with CH2Cl2 (100 mL)
- additionSaturated aq. K2CO3 (150 mL) was added to the aqueous phase
- extractionThe product was extracted with CH2Cl2 (2×100 mL), extracts
- dry with materialwere dried over Na2SO4
- customevaporated
- customThe residue was dried under vacuum
出典と根拠
- ORDレコード
- ord-302ca1e54f8f445f8d8783930243f86e
- 出典データセット
- uspto-grants-2014_04
- 特許番号
- US08686005B2
反応ノート
読み込み中…