Ethylene Glycol → 2-Amino-5-methylbenzene-1-thiol
반응식
NC1[S:3][C:4]2[CH:10]=[C:9]([CH3:11])[CH:8]=[CH:7][C:5]=2[N:6]=1.C(O)CO.[OH-].[K+].C1(C)C=CC=CC=1>C(O)(=O)C>[CH3:11][C:9]1[CH:8]=[CH:7][C:5]([NH2:6])=[C:4]([SH:3])[CH:10]=1참가 물질
6
실험 절차
A mixture of 2-amino-6-methylbenzothiazole (15 g, 91.3 mmol), ethylene glycol (22.26 g, 0.36 mol) and 50% w/v KOH (180 ml) was heated under reflux for 62 h. On cooling to room temperature, toluene (60 ml) was added and the reaction mixture was cooled in an ice-bath and acidified with acetic acid (final pH 5-6). The reaction mixture was extracted with toluene (5×300 ml) and the combined organic extracts were washed with brine (2×200 ml), dried (MgSO4) and the solvent removed under reduced pressure to give the title compound (11.1 g, 86%) as a yellow solid which was used without further purification.
후처리
- temperaturewas heated
- temperatureunder reflux for 62 h
- temperaturethe reaction mixture was cooled in an ice-bath
- extractionThe reaction mixture was extracted with toluene (5×300 ml)
- washthe combined organic extracts were washed with brine (2×200 ml)
- dry with materialdried (MgSO4)
- customthe solvent removed under reduced pressure
출처 및 근거
- ORD 기록
- ord-3fddf22e12cf4bc68ed7a1a09f836cac
- 출처 데이터셋
- uspto-grants-2014_11
- 특허 번호
- US08895313B2
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