Sulfuric Acid → N-tert-Butyl-3,3-dimethyl-2-oxobutanamide

HRID 27838

반응식

HRID 27838 반응식
[C:1]([C:7]#[N:8])(=[O:6])[C:2]([CH3:5])([CH3:4])[CH3:3].S(=O)(=O)(O)[OH:10].[CH3:14][C:15](=[CH2:17])[CH3:16]>C(O)(=O)C>[C:15]([NH:8][C:7](=[O:10])[C:1]([C:2]([CH3:5])([CH3:4])[CH3:3])=[O:6])([CH3:16])([CH3:14])[CH3:17]

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 8255IsobutyleneHCID 945273,3-Dimethyl-2-oxobutanenitrile

생성물 1

HCID 13355144N-tert-Butyl-3,3-dimethyl-2-oxobutanamide수율 87%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

There were present in a stirrer apparatus protected against moisture 111 grams (1.0 mole) of pivaloyl cyanide, 150 grams (1.5 moles) of concentrated sulfuric acid and 150 ml of glacial acetic acid and there were led in during one hour under stirring at 0°-5° C.112 grams (2.0 moles) of isobutylene. Then the mixture was warmed up to room temperature and stirred further for 4 hours. Then the mixture was poured on 500 grams of ice and after thorough stirring the precipitated amide was filtered off with suction. After the drying in the vacuum drying cabinet, there were isolated 161 grams of analytically pure trimethyl pyruvic acid-N-t-butylamide which corresponds to a yield of 87% based on the acyl cyanide employed. The amide has a melting point of 65° C.

후처리

  1. customThere were present in a stirrer
  2. customwere led in during one hour
  3. stirringstirred further for 4 hours
  4. filtrationwas filtered off with suction
  5. customAfter the drying in the vacuum drying cabinet

출처 및 근거

ORD 기록
ord-9689268751db44e2befdb5fba3d7f975
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04224226

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