1,3-Dibromopropane → HCID 10879224、化合物
反応式
[OH:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][CH:3]=1.[Br:10][CH2:11][CH2:12][CH2:13]Br.C([O-])([O-])=O.[Cs+].[Cs+]>C(#N)C>[Br:10][CH2:11][CH2:12][CH2:13][O:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][CH:3]=1参加物
5
実験手順
To a solution of 4-hydroxybenzonitrile (0.109 g, 0.913 mmol) in acetonitrile (4 mL) was added 1,3-dibromopropane (0.930 mL, 9.16 mmol) followed by Cs2CO3 (0.439 g, 1.35 mmol). The reaction mixture was stirred for 24 h and then concentrated under vacuum. The resulting residue was treated with H2O (4 mL) and extracted with DCM (8 mL). The organic layer was dried through a phase separator and concentrated under vacuum. The residue was taken up in DMSO and purified by preparatory HPLC (without TFA) to give the title compound (0.156 g, 71.4%). EI-MS Rt (2.10 min).
後処理
- concentrationconcentrated under vacuum
- additionThe resulting residue was treated with H2O (4 mL)
- extractionextracted with DCM (8 mL)
- customThe organic layer was dried through a phase separator
- concentrationconcentrated under vacuum
- custompurified by preparatory HPLC (without TFA)
出典と根拠
- ORDレコード
- ord-77fec98d8dc5494f8eeac1b4e16914fe
- 出典データセット
- uspto-grants-2014_10
- 特許番号
- US08853404B2
反応ノート
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