Hydrochloric Acid → 2-Amino-5-nitrobenzenethiol
反応式
[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]参加物
6
実験手順
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).
後処理
- 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
出典と根拠
- ORDレコード
- ord-6c5b3c41325c4c05a926a6970d2485b8
- 出典データセット
- uspto-grants-2012_01
- 特許番号
- US08106043B2
反応ノート
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