Bromine → 6-Bromo-2,4-dimethylpyridin-3-amine
反応式
[CH3:1][C:2]1[C:7]([NH2:8])=[C:6]([CH3:9])[CH:5]=[CH:4][N:3]=1.[Br:10]Br>C(Cl)Cl>[Br:10][C:4]1[N:3]=[C:2]([CH3:1])[C:7]([NH2:8])=[C:6]([CH3:9])[CH:5]=1参加物
4
実験手順
To a solution of 2,4-dimethylpyridin-3-amine (2.0 g, 16 mmol) in CH2Cl2 (20 mL), was added a solution of bromine (3.16 g; 20 mmol) in CH2Cl2 (5 mL) at 0° C. for 5 min. The reaction was concentrated under vacuum. The reaction was poured into H2O (50 mL), extracted with CH2Cl2, washed with Na2SO3 solution, and dried over MgSO4. The CH2Cl2 was concentrated under vacuum to afford the crude compound. The crude was purified over SiO2 to afford to give 6-bromo-2,4-dimethylpyridin-3-amine. 1HNMR (CDCl3, 400 MHz) δ 2.10 (s, 3H), 2.31 (s, 3H), 4.85-5.10 (b, 2H), 7.05 (s, 1H). Exact mass calculated for C7H9BrN2 201.06. found 202.3 (MH+).
後処理
- concentrationThe reaction was concentrated under vacuum
- additionThe reaction was poured into H2O (50 mL)
- extractionextracted with CH2Cl2
- washwashed with Na2SO3 solution
- dry with materialdried over MgSO4
- concentrationThe CH2Cl2 was concentrated under vacuum
- customto afford the crude compound
- customThe crude was purified over SiO2
- customto afford
出典と根拠
- ORDレコード
- ord-2c4a5becfc7546ecb8a27cf100868a25
- 出典データセット
- uspto-grants-2013_01
- 特許番号
- US08362248B2
反応ノート
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