Ammonium Chloride → 3-Amino-2-methylbenzonitrile
反応式
[CH3:1][C:2]1[C:9]([N+:10]([O-])=O)=[CH:8][CH:7]=[CH:6][C:3]=1[C:4]#[N:5].[Cl-].[NH4+]>O1CCCC1.CO.[Zn]>[NH2:10][C:9]1[C:2]([CH3:1])=[C:3]([CH:6]=[CH:7][CH:8]=1)[C:4]#[N:5]参加物
6
実験手順
To a mixture of 2-methyl-3-nitrobenzonitrile (5.50 g, 33.9 mmol) and ammonium chloride (25.4 g, 475 mmol) in tetrahydrofuran (100 mL) and methanol (100 mL) at 0° C. was added zinc dust (31.1 g, 475 mmol) in portions. The mixture was stirred at room temperature for 2 hr. The insoluble material was removed by suction filtration through CELITE®, and the filtrate was concentrated under vacuum. The residue was diluted with water (50 mL) and extracted with CH2Cl2 (4×100 mL). The combined extract was dried over anhydrous MgSO4. Removal of solvent under vacuum provided the desired product (4.19 g, 31.7 mmol, 93% yield) as a white solid.
後処理
- customThe insoluble material was removed by suction filtration through CELITE®
- concentrationthe filtrate was concentrated under vacuum
- additionThe residue was diluted with water (50 mL)
- extractionextracted with CH2Cl2 (4×100 mL)
- extractionThe combined extract
- dry with materialwas dried over anhydrous MgSO4
- customRemoval of solvent under vacuum
出典と根拠
- ORDレコード
- ord-d92ae08ba65d46718990ad7be9884318
- 出典データセット
- uspto-grants-2014_04
- 特許番号
- US08685969B2
反応ノート
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