Ammonia → HCID 18180211、化合物
反応式
Cl[C:2]1[C:7]([Br:8])=[N:6][CH:5]=[C:4]([NH2:9])[N:3]=1.[NH3:10]>C(O)C>[NH2:10][C:2]1[C:7]([Br:8])=[N:6][CH:5]=[C:4]([NH2:9])[N:3]=1参加物
4
反応条件
- 温度
- 160 °C
実験手順
A suspension of 2-chloro-3-bromo-6-aminopyrazine (15 g, 0.072 mole) in absolute ethanol (150 ml) and 0.880 ammonia (375 ml) was stirred and heated in an autoclave at 160° C. and 20 atm. for 16 hrs. The cooled mixture was evaporated in vacuo and extracted with hot methanol (3×100 ml). The combined methanol extracts were evaporated in vacuo. The residue was dissolved in hot chloroform, dried over anhydrous magnesium sulphate, filtered and the filtrate evaporated in vacuo. The residue was triturated with 40-60° C. petroleum ether, filtered, and dried in vacuo. Yield 5.51 g (40%), M.p. 176-178° C.
後処理
- customThe cooled mixture was evaporated in vacuo
- extractionextracted with hot methanol (3×100 ml)
- customThe combined methanol extracts were evaporated in vacuo
- dissolutionThe residue was dissolved in hot chloroform
- dry with materialdried over anhydrous magnesium sulphate
- filtrationfiltered
- customthe filtrate evaporated in vacuo
- customThe residue was triturated with 40-60° C. petroleum ether
- filtrationfiltered
- customdried in vacuo
出典と根拠
- ORDレコード
- ord-984a243b4b0a42e5828df20265ddba3d
- 出典データセット
- uspto-grants-2001_07
- 特許番号
- US06255307B1
反応ノート
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