Sulfuric Acid → HCID 10307918、化合物

HRID 2194933ノート

反応式

HRID 2194933 の反応式
S(=O)(=O)(O)O.[NH2:6][C:7]1[CH:12]=[CH:11][C:10]([CH3:13])=[CH:9][CH:8]=1.[N+]([O-])(O)=O.N[C:19]([NH2:21])=O.[C:22]([O:25]CC)(=[O:24])C.[CH3:28]CCCCC>[OH-].[Na+]>[NH:6]1[C:7]2[C:12](=[CH:11][C:10]([CH:13]([CH3:28])[C:22]([OH:25])=[O:24])=[CH:9][CH:8]=2)[CH:19]=[N:21]1

参加物

6

反応物 4

HCID 1118Sulfuric AcidHCID 7813p-ToluidineHCID 31295Urea nitrateHCID 21226206Ethyl acetate hexane

生成物 1

HCID 10307918HCID 10307918、化合物収率 88%

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

Sulfuric acid (365.8 g, 3.73 mol, 10 eq) was added drop wise to p-toluidine (40 g, 0.37 mol) at it and stirred the contents to obtain a clear solution. Then Urea nitrate (45.5 g, 0.37 mol, 1 eq) was added at 0-10° C. and stirred the reaction mass for 30 min at the same temperature. Progress of the reaction was monitored by TLC (30% ethyl acetate/hexane, Rf˜0.5). On completion of the reaction, reaction mixture was quenched with ice water and the solid formed was filtered. Solid obtained was taken in 20% NaOH solution (up to pH˜12) and filtered. Washed the solid and dried to yield the required product as an yellow colored solid (50 g, 88% yield).

後処理

  1. customto obtain a clear solution
  2. stirringstirred the reaction mass for 30 min at the same temperature
  3. customOn completion of the reaction, reaction mixture
  4. customwas quenched with ice water
  5. customthe solid formed
  6. filtrationwas filtered
  7. customSolid obtained
  8. filtrationfiltered
  9. washWashed the solid
  10. customdried

出典と根拠

ORDレコード
ord-df32e1563be546e3934f070a7db93dec
出典データセット
uspto-grants-2012_12
特許番号
US08334315B2

反応ノート

読み込み中…