Chloroacetyl chloride → 5-Hydroxy-2H-1,4-benzoxazin-3(4H)-one
反応式
[NH2:1][C:2]1[C:7]([OH:8])=[CH:6][CH:5]=[CH:4][C:3]=1[OH:9].Cl[CH2:11][C:12](Cl)=[O:13].C([O-])([O-])=O.[K+].[K+]>CN(C=O)C.O>[OH:8][C:7]1[C:2]2[NH:1][C:12](=[O:13])[CH2:11][O:9][C:3]=2[CH:4]=[CH:5][CH:6]=1参加物
6
実験手順
To a solution of 2-aminobenzene-1,3-diol (2.00 g, 16.0 mmol) and TEA (1.94 g, 19.2 mmol) in anhydrous DMF (30 mL) was added 2-chloroacetyl chloride (1.81 g, 16.0 mmol). After 16 h, K2CO3 (2.65 g, 19.2 mmol) was added and the reaction mixture was stirred for another 16 h. The mixture was diluted with water and extracted with DCM. The combined organic extracts were washed with water, brine, the combined organic extracts dried over sodium sulfate, filtered and concentrated. The crude product was purified by column chromatography. (1.7 g, yield 65%).
後処理
- extractionextracted with DCM
- washThe combined organic extracts were washed with water, brine
- dry with materialthe combined organic extracts dried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated
- customThe crude product was purified by column chromatography
出典と根拠
- ORDレコード
- ord-1aeac3c024554e848c9652d36b8bfe13
- 出典データセット
- uspto-grants-2015_12
- 特許番号
- US09221794B2
反応ノート
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