Chloroacetaldehyde → HCID 90412925、化合物
反応式
[NH2:1][C:2]1[N:7]=[C:6]([C:8]([OH:10])=[O:9])[C:5]([CH3:11])=[CH:4][CH:3]=1.[OH-].[Na+].Cl[CH2:15][CH:16]=O>O>[CH3:11][C:5]1[CH:4]=[CH:3][C:2]2[N:7]([CH:15]=[CH:16][N:1]=2)[C:6]=1[C:8]([OH:10])=[O:9]参加物
5
反応条件
- 温度
- 150 °C
実験手順
To the title compound of Step A (340 mg, 2.2 mmol) in H2O (7 mL) was added 1M aq. NaOH (2.2 mL, 2.2 mmol) and chloroacetaldehyde (210 μL, 3.4 mmol) and the reaction mixture heated in a microwave reactor at 150° C. for 2 h. Additional 1M aq. NaOH (2.2 mL, 2.2 mmol) and chloroacetaldehyde (210 μL, 3.4 mmol) were added and heating continued at 150° C. for 2 h. The reaction was purified via prep HPLC to give the title compound (282 mg, 72%). MS (ESI) mass calcd. for C9H8N2O2, 176.1; m/z found 177.0 [M+H]+.
後処理
- temperatureheating
- customThe reaction was purified via prep HPLC
出典と根拠
- ORDレコード
- ord-70218fa18f3e41579a0c2898fc8eb921
- 出典データセット
- uspto-grants-2015_06
- 特許番号
- US09062078B2
反応ノート
読み込み中…