Nitric Acid → HCID 13388013、化合物
反応式
[F:1][C:2]1[CH:11]=[CH:10][CH:9]=[CH:8][C:3]=1[CH:4]([C:6]#[N:7])[CH3:5].[N+:12]([O-])([OH:14])=[O:13]>>[F:1][C:2]1[CH:11]=[CH:10][C:9]([N+:12]([O-:14])=[O:13])=[CH:8][C:3]=1[CH:4]([C:6]#[N:7])[CH3:5]参加物
3
実験手順
To 24 g of 2-fluoro-α-methylbenzyl cyanide was added dropwise 40 ml of fuming nitric acid while maintaining the temperature 0°-5° C. After addition, the mixture was gradually warmed up to room temperature, poured into ice-water and extracted with ether. The ether layer was washed with water and dried over anhydrous magnesium sulfate and the solvent was evaporated off. The crude crystals obtained were recrystallized from benzene--n-hexane to afford 25.8 g of 2-fluoro-α-methyl-5-nitrobenzyl cyanide, m.p. 55°-56° C.
後処理
- temperaturewhile maintaining the temperature 0°-5° C
- additionAfter addition
- extractionextracted with ether
- washThe ether layer was washed with water
- dry with materialdried over anhydrous magnesium sulfate
- customthe solvent was evaporated off
- customThe crude crystals obtained
- customwere recrystallized from benzene
出典と根拠
- ORDレコード
- ord-d6aae3d2d3384f8598b908efadfc55c1
- 出典データセット
- uspto-grants-1985_12
- 特許番号
- US04557871
反応ノート
読み込み中…