1,3-Dibromopropane → 5-(3-Bromopropoxy)benzo[d]thiazole
反応式
[S:1]1[C:5]2[CH:6]=[CH:7][C:8]([OH:10])=[CH:9][C:4]=2[N:3]=[CH:2]1.[Br:11][CH2:12][CH2:13][CH2:14]Br.C([O-])([O-])=O.[K+].[K+]>CCO>[Br:11][CH2:12][CH2:13][CH2:14][O:10][C:8]1[CH:7]=[CH:6][C:5]2[S:1][CH:2]=[N:3][C:4]=2[CH:9]=1参加物
5
実験手順
A mixture of intermediate 25 (1 g, 6.6 mmol), 1,3-dibromopropane (1.83 mL, 18 mmol), anhydrous K2CO3 (828 mg, 6.0 mmol) and EtOH (20 mL) was heated to reflux and stirred overnight. The yellow solid was filtered and purified by column chromatography (elution with PE/EtOAc=3:1) to afford 5-(3-bromopropoxy)benzo[d]thiazole (intermediate 27) (543 mg, 33%) as a yellow oil.
後処理
- temperaturewas heated
- temperatureto reflux
- filtrationThe yellow solid was filtered
- custompurified by column chromatography (elution with PE/EtOAc=3:1)
出典と根拠
- ORDレコード
- ord-87fab5765c9e4b60bdfa7972a25b0bb7
- 出典データセット
- uspto-grants-2015_10
- 特許番号
- US09156822B2
反応ノート
読み込み中…