Sulfuric Acid → phenylglyoxylic-N-t-butylamide

HRID 67199

반응식

HRID 67199 반응식
[C:1]([C:9]#[N:10])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CO[C:13]([CH3:16])([CH3:15])[CH3:14].S(=O)(=O)(O)[OH:18]>C(O)(=O)C>[C:13]([NH:10][C:9](=[O:18])[C:1]([C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)=[O:8])([CH3:16])([CH3:15])[CH3:14]

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 11953PhenylglyoxylonitrileHCID 15413tert-Butyl methyl ether

생성물 1

HCID 10965642phenylglyoxylic-N-t-butylamide

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

32.8 g (0.25 mole) of benzoyl cyanide, dissolved in 22 g (0.25 mole) of t-butyl methyl ether were added to a reaction mixture, which had been initially introduced into the reaction vessel, consisting of 37.5 g of concentrated sulphuric acid and 52.5 g of glacial acetic acid at 20° to 30° C. in the course or 30 minutes. After subsequently stirring the reaction mixture at room temperature for 2 hours, it was poured onto 125 g of ice and stirred thoroughly. The product which precipitates was filtered off, washed with water and dried. 45.6 g (88.9% of theory) of analytically pure phenylglyoxylic acid N-tert.-butylamide with a melting point of 78° C. and a content of >99% (determined by gas chromatography) were obtained.

후처리

  1. additionwere added to a reaction mixture, which
  2. additionhad been initially introduced into the reaction vessel
  3. stirringstirred thoroughly
  4. customThe product which precipitates
  5. filtrationwas filtered off
  6. washwashed with water
  7. customdried

출처 및 근거

ORD 기록
ord-fb71ed52c18c4352b397111daaadeb49
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04345100

연결된 노트

불러오는 중…