O-Cresol → 1-(3-Bromopropoxy)-2-methylbenzene
反応式
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[OH:8].[Br:9][CH2:10][CH2:11][CH2:12]Br.C([O-])([O-])=O.[Cs+].[Cs+]>C(#N)C>[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[O:8][CH2:12][CH2:11][CH2:10][Br:9]参加物
5
実験手順
To a solution of 2-methylphenol (0.0954 g, 0.924 mmol) in acetonitrile (4 mL) was added 1,3-dibromopropane (1.00 mL, 9.85 mmol) followed by Cs2CO3 (0.469 g, 1.44 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 (0.0934 g, 44.1%). EI-MS Rt (2.45 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-c1c3893d431a425d9a2c06d74a113c51
- 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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