1,4-Dimethyl 2-oxobutanedioate → HCID 178498583、化合物
反応式
[NH2:1][C:2]1[N:6]=[C:5]([CH3:7])[NH:4][N:3]=1.O=[C:9]([CH2:14][C:15](OC)=[O:16])[C:10]([O:12][CH3:13])=[O:11]>C(O)(=O)C>[OH:16][C:15]1[N:3]2[N:4]=[C:5]([CH3:7])[N:6]=[C:2]2[N:1]=[C:9]([C:10]([O:12][CH3:13])=[O:11])[CH:14]=1参加物
4
実験手順
3-Amino-5-methyl-1H-s-triazole (112 mg) and 320 mg of dimethyl 2-oxo-succinate are dissolved in 5 ml of glacial acetic acid. After boiling under reflux for 22 hours the solvent is distilled off in a vacuum. The residue is suspended in warm methanol. After cooling the product is filtered off and washed several times with methanol. After drying in a high vacuum there are obtained 73 mg of methyl 7-hydroxy-2-methyl-s-triazolo[1,5-a]pyrimidine-5-carboxylate as a beige powder, m.p.>220° C.
後処理
- temperatureunder reflux for 22 hours the solvent
- distillationis distilled off in a vacuum
- temperatureAfter cooling the product
- filtrationis filtered off
- washwashed several times with methanol
- customAfter drying in a high vacuum
出典と根拠
- ORDレコード
- ord-0314e06e4d814d7e95b908f836260812
- 出典データセット
- uspto-grants-1995_08
- 特許番号
- US05438052
反応ノート
読み込み中…