Sulfuric Acid → HCID 10307918, 화합물

HRID 2194933노트

반응식

HRID 2194933 반응식
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

참가 물질

6

반응물 4

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

생성물 1

HCID 10307918HCID 10307918, 화합물수율 88%

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-df32e1563be546e3934f070a7db93dec
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08334315B2

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