Sulfuric Acid → N-(1,1-Dimethyl-2-phenylethyl)formamide

HRID 76148

반응식

HRID 76148 반응식
[C-]#[N:2].[Na+].S(=O)(=O)(O)O.[C-]#N.[Na+].C[C:13]([OH:15])=O.[CH3:16][C:17](O)([CH3:25])[CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.C([O-])([O-])=O.[Na+].[Na+]>C(O)(=O)C>[CH3:16][C:17]([NH:2][CH:13]=[O:15])([CH3:25])[CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1

참가 물질

7

반응물 5

HCID 1118Sulfuric AcidHCID 75312-Methyl-1-phenyl-2-propanolHCID 8929Sodium CyanideHCID 10340Sodium CarbonateHCID 23665388NaCN AcOH

생성물 1

HCID 104077N-(1,1-Dimethyl-2-phenylethyl)formamide

시약·촉매·용매 1

HCID 176Acetic Acid용매3회

실험 절차

11.3 g (230 mmol) NaCN are added to 60 mL AcOH. A combination of 30 mL AcOH and 60 mL concentrated sulfuric acid is carefully dropped into the NaCN/AcOH mixture while maintaining the temperature below 20° C. Then 30 mL (195 mmol) 2-methyl-1-phenyl-2-propanol, in 30 mL acetic acid, are added dropwise to the reaction mixture, again keeping the temperature below 20° C. After having finished the addition, the reaction mixture is stirred for an additional hour at r.t., poured onto ice water and is finally neutralised with an aq. Na2CO3 solution. The resulting mixture is extracted with diethylether. The organic layer is dried with MgSO4, filtered and the solvent is removed under reduced pressure. The crude product is used without further purification.

후처리

  1. temperaturewhile maintaining the temperature below 20° C
  2. customthe temperature below 20° C
  3. additionthe addition
  4. additionpoured onto ice water
  5. extractionThe resulting mixture is extracted with diethylether
  6. dry with materialThe organic layer is dried with MgSO4
  7. filtrationfiltered
  8. customthe solvent is removed under reduced pressure
  9. customThe crude product is used without further purification

출처 및 근거

ORD 기록
ord-af1770bfb9894dc1acb4a28a3c24a4bd
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08835472B2

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