Sulfuric Acid → N-[1,1-dimethyl-2-(2,4,6-trimethylphenyl)ethyl]formamide

HRID 966102노트

반응식

HRID 966102 반응식
[C-]#[N:2].[K+].S(=O)(=O)(O)O.[CH3:9][C:10](O)([CH3:21])[CH2:11][C:12]1[C:17]([CH3:18])=[CH:16][C:15]([CH3:19])=[CH:14][C:13]=1[CH3:20].[C:23](=[O:26])([O-])[O-].[Na+].[Na+]>C(O)(=O)C>[CH3:9][C:10]([NH:2][CH:23]=[O:26])([CH3:21])[CH2:11][C:12]1[C:17]([CH3:18])=[CH:16][C:15]([CH3:19])=[CH:14][C:13]=1[CH3:20]

참가 물질

6

반응물 4

HCID 1118Sulfuric AcidHCID 9032Potassium CyanideHCID 10340Sodium CarbonateHCID 223145482-Methyl-1-(2,4,6-trimethylphenyl)propan-2-ol

생성물 1

HCID 22314552N-[1,1-dimethyl-2-(2,4,6-trimethylphenyl)ethyl]formamide

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

실험 절차

90 mL of glacial acetic acid and 33 g of potassium cyanide are combined while cooling with ice. 90 mL of sulfuric acid and 90 mL of glacial acetic acid are then added dropwise at 20° C. 65 g of 2-methyl-1-(2,4,6-trimethylphenyl)propan-2-ol is slowly added to the solution at constant temperature. After the addition has ended, the mixture is stirred for a further hour. The mixture is poured onto ice water, neutralized with sodium carbonate solution, and extracted with diethyl ether. The solvent is distilled off under reduced pressure and the residue is fractionally distilled. Yield: 55 g (74%); bp0.1: 155° C.

후처리

  1. temperaturewhile cooling with ice
  2. additionAfter the addition
  3. additionThe mixture is poured onto ice water
  4. extractionextracted with diethyl ether
  5. distillationThe solvent is distilled off under reduced pressure
  6. distillationthe residue is fractionally distilled
  7. custom155° C.

출처 및 근거

ORD 기록
ord-68ba0bacb06145f1b0b9d0110ba4a991
출처 데이터셋
uspto-grants-2005_10
특허 번호
US06951888B2

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