Methylamine → 1-(4-Bromophenyl)-2-methylaminoethanol
反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[CH2:10][O:9]2)=[CH:4][CH:3]=1.[CH3:11][NH2:12]>>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([OH:9])[CH2:10][NH:12][CH3:11])=[CH:4][CH:3]=1参加物
3
実験手順
A solution of 2-(4-bromophenyl)-oxirane (0.5 g, 2.51 mmol) in methylamine (6.6 ml, 33% by volume in ethanol, 25.12 mmol) was stirred at room temperature under an atmosphere of nitrogen. After 18 hours the solvent was removed in vacuo and the residue was purified over flash silica eluting with dichloromethane: methanol: acetic acid:water (120:15:3:2) to afford the desired compound as the acetic acid salt. Further purification over a Phenomenex_Strata_SCX column eluting with methanol followed by 2N ammonia in methanol gave the desired product. LC/MS: (PS-B3) Rt 2.52 [M+H]+ 230.
後処理
- customAfter 18 hours the solvent was removed in vacuo
- customthe residue was purified over flash silica eluting with dichloromethane: methanol: acetic acid:water (120:15:3:2)
出典と根拠
- ORDレコード
- ord-2a0c762d7dbf4ed292e806016539b26c
- 出典データセット
- uspto-grants-2012_08
- 特許番号
- US08247576B2
反応ノート
読み込み中…