Nitric Acid → HCID 13388013、化合物

HRID 637614ノート

反応式

HRID 637614 の反応式
[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

  1. temperaturewhile maintaining the temperature 0°-5° C
  2. additionAfter addition
  3. extractionextracted with ether
  4. washThe ether layer was washed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customthe solvent was evaporated off
  7. customThe crude crystals obtained
  8. 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…