Hydrochloric Acid → 3-(2-Amino-3-methylthiocarbamoyloxypropoxy)-5-chloro-1,2-benzoisoxazole hydrochloride
반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][N:8]=[C:7]([O:10][CH2:11][CH:12]([NH:19]C(OC(C)(C)C)=O)[CH2:13][O:14][C:15](=[S:18])[NH:16][CH3:17])[C:6]=2[CH:27]=1.O1CCOCC1.Cl.CC(O)C>CO>[ClH:1].[NH2:19][CH:12]([CH2:13][O:14][C:15](=[S:18])[NH:16][CH3:17])[CH2:11][O:10][C:7]1[C:6]2[CH:27]=[C:2]([Cl:1])[CH:3]=[CH:4][C:5]=2[O:9][N:8]=1참가 물질
6
실험 절차
To a solution of 0.4 g of 5-chloro-3-(2-tert-butoxycarbonylamino-3-methylthiocarbamoyloxypropoxy)-1,2-benzoisoxazole in 10 ml of methanol is added 5 ml of a dioxane solution (3.2N) of hydrogen chloride at room temperature, and they are subjected to reaction at the same temperature for three hours, after which the solvent is removed by distillation under reduced pressure. To the residue obtained is added 3 ml of 2-propanol, and the crystals precipitated are collected by filtration, to obtain 0.22 g of pale yellow, crystalline 3-(2-amino-3-methylthiocarbamoyloxypropoxy)-5-chloro-1,2-benzoisoxazole hydrochloride having a melting point of 198.8°-199.2° C. (decomp.).
후처리
- customthey are subjected to reaction at the same temperature for three hours
- customafter which the solvent is removed by distillation under reduced pressure
- customTo the residue obtained
- customthe crystals precipitated
- filtrationare collected by filtration
출처 및 근거
- ORD 기록
- ord-f79c01ee8c7d48ef8f1fc8bdf01e255d
- 출처 데이터셋
- uspto-grants-1996_11
- 특허 번호
- US05578627
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