Hydrogen Bromide → HCID 68902424、化合物
反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([C:10](=O)[CH2:11][S:12][C:13]#[N:14])=[CH:6][CH:5]=1)([O-:3])=[O:2].[BrH:16].[OH-].[Na+].O>C(O)(=O)C>[Br:16][C:13]1[S:12][CH:11]=[C:10]([C:7]2[CH:8]=[CH:9][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][CH:6]=2)[N:14]=1参加物
6
実験手順
2-(4-Nitrophenyl)-2-oxoethyl thiocyanate (3.0 g; 15.4 mmol) and 50 mL of 30% HBr in acetic acid were stirred at room temperature under nitrogen overnight. The yellow paste was neutralized with 60 mL of 2N NaOH and 60 mL of H2O. The residue was collected by suction filtration. Purification of the residue on silica gel using a stepwise gradient of 5-50% ethyl acetate:hexane gave 2-bromo-4-(4-nitrophenyl)-1,3-thiazole (2.0 g, 45%), MS (ES) m/z 286[M+H]+.
後処理
- filtrationThe residue was collected by suction filtration
- customPurification of the residue on silica gel using a stepwise gradient of 5-50% ethyl acetate
出典と根拠
- ORDレコード
- ord-035e9b0379814ac0b00bc3e4b82f5040
- 出典データセット
- uspto-grants-2009_11
- 特許番号
- US07618990B2
反応ノート
読み込み中…