Chloroacetyl chloride → 5-Hydroxy-2H-1,4-benzoxazin-3(4H)-one
반응식
[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]=1참가 물질
6
실험 절차
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%).
후처리
- 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
출처 및 근거
- ORD 기록
- ord-1aeac3c024554e848c9652d36b8bfe13
- 출처 데이터셋
- uspto-grants-2015_12
- 특허 번호
- US09221794B2
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