Hydrochloric Acid → 2-Amino-5-nitrobenzenethiol
반응식
[N+:1]([C:4]1[CH:12]=[CH:11][C:7]2[N:8]=C[S:10][C:6]=2[CH:5]=1)([O-:3])=[O:2].O.NN.Cl>C(O)C.O>[NH2:8][C:7]1[CH:11]=[CH:12][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][C:6]=1[SH:10]참가 물질
6
실험 절차
To a stirred suspension of 6-nitrobenzo[d]thiazole (1.64 g, 9.10 mmol) in ethanol (16 mL) was added hydrazine hydrate (2.66 mL, 54.6 mmol). The resulting dark solution was stirred overnight at room temperature. The mixture was then diluted with water and slowly acidified with 3 M HCl, giving a yellow suspension. The mixture was then extracted with dichloromethane. The combined organics were dried, filtered, and concentrated, giving a yellow solid, used directly in the subsequent reaction. 1H NMR (DMSO-d6) δ 8.09 (brs, 1H), 7.87 (d, J=8.7 Hz, 1H), 6.74 (d, J=9.0 Hz, 1H), 6.27 (brs, 2H); MS-EI: (m/z, %) 170 (M+, 100), 140 (28), 124 (35).
후처리
- customgiving a yellow suspension
- extractionThe mixture was then extracted with dichloromethane
- customThe combined organics were dried
- filtrationfiltered
- concentrationconcentrated
- customgiving a yellow solid
- customused directly in the subsequent reaction
출처 및 근거
- ORD 기록
- ord-6c5b3c41325c4c05a926a6970d2485b8
- 출처 데이터셋
- uspto-grants-2012_01
- 특허 번호
- US08106043B2
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