Sodium Hydroxide → N-phenyl-1H-imidazol-2-amine
反応式
C(O[CH:4](OCC)[CH2:5][NH:6][C:7]([NH:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)=[NH:8])C.[OH-].[Na+]>Cl>[C:10]1([NH:9][C:7]2[NH:8][CH:4]=[CH:5][N:6]=2)[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1参加物
4
実験手順
The guanidine (b) was dissolved in HCl (5 mL, 6 M) at 0° C. and then stirred for 2 h. After the starting material was consumed, NaOH (25%) was added until a precipitate formed. This mixture was stirred for 30 min. The reaction was then poured into NaOH (0.5 M), extracted with CH2Cl2, dried and concentrated. Flash chromatography afforded (c) (0.95 g, 50%). 1H NMR (500 MHz, DMSO-d6) δ 8.58 (s, br, 1H), 7.34-6.74 (m, 5H), 6.68 (s, 2H), 6.62 (br, 2H), 3.82 (s, 6H), 3.73 (s, 3H). MS: 157.6 (M−H)−; 160.0 (M+H)+.
後処理
- customAfter the starting material was consumed
- additionNaOH (25%) was added until a precipitate
- customformed
- stirringThis mixture was stirred for 30 min
- extractionextracted with CH2Cl2
- customdried
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-2cd5d24c2cfe43da8db53b5b7ce5c9c3
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09447049B2
反応ノート
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