Ethyl bromoacetate → 7-Bromo-2H-(1,4)-benzothiazin-3(4h)-one
反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([Br:8])=[CH:4][C:3]=1[SH:9].Br[CH2:11][C:12](OCC)=[O:13].C(=O)(O)[O-].[Na+]>CN(C=O)C.O>[Br:8][C:5]1[CH:6]=[CH:7][C:2]2[NH:1][C:12](=[O:13])[CH2:11][S:9][C:3]=2[CH:4]=1参加物
6
実験手順
A mixture of 2-amino-5-bromo-benzenethiol (20 g, 0.1 mol), ethyl bromoacetate (19 g, 0.1 mol), and sodium bicarbonate (8.8 g, 0.1 mol) in DMF (200 ml) was heated to reflux for 2 hours. The mixture was diluted with water and extracted with ethyl acetate (2×100 mL). The combined organic extracts were washed with water, then brine, dried (MgSO4) and evaporated to obtain the crude 7-bromo-4H-benzo[1,4]thiazin-3-one (20 g, 82%). A small portion of sample was recrystallized from ethanol to afford pure 7-bromo-4H-benzo[1,4]thiazin-3-one: mp 212-213° C.; MS (EI) m/z 243/245 (M+).
後処理
- temperaturewas heated
- temperatureto reflux for 2 hours
- extractionextracted with ethyl acetate (2×100 mL)
- washThe combined organic extracts were washed with water
- dry with materialbrine, dried (MgSO4)
- customevaporated
出典と根拠
- ORDレコード
- ord-e50172ae9f6142a88197f249cfba527d
- 出典データセット
- uspto-grants-2004_09
- 特許番号
- US06794373B2
反応ノート
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