Methyl propiolate → HCID 178498875, 화합물

HRID 235968

반응식

HRID 235968 반응식
[C:1]([O:5][CH3:6])(=[O:4])[C:2]#[CH:3].[CH3:7][O:8][C:9]1[CH:18]=[CH:17][C:12]([C:13](=[N:15]O)[NH2:14])=[CH:11][CH:10]=1>CO>[C:1]([C:2]1[N:14]=[C:13]([C:12]2[CH:17]=[CH:18][C:9]([O:8][CH3:7])=[CH:10][CH:11]=2)[NH:15][CH:3]=1)([O:5][CH3:6])=[O:4]

참가 물질

4

반응물 2

HCID 13536Methyl propiolateHCID 21471p-Methoxybenzamidoxime

생성물 1

HCID 178498875HCID 178498875, 화합물수율 30.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of methyl propiolate (25.4 g, 0.3 mol), p-methoxybenzamidoxime (50 g, 0.3 mol) and CH3OH (700 ml) was heated at reflux with stirring. After 8 hours, the reaction mixture was concentrated to dryness, and the residue treated with diphenyl ether (300 ml) and heated at reflux. After 2.5 hours, the reaction mixture was poured in C6H14 (2 L) and allowed to stand. The C6H14 was decanted off and the residue chromatographed on silica gel. The product was eluted with 2% CH3OH--CHCl3 to yield 21 g (30%) of 63; m.p. 188°-90° C. (trituration with Et2O).

후처리

  1. temperatureat reflux
  2. concentrationthe reaction mixture was concentrated to dryness
  3. additionthe residue treated with diphenyl ether (300 ml)
  4. temperatureheated
  5. temperatureat reflux
  6. waitAfter 2.5 hours
  7. additionthe reaction mixture was poured in C6H14 (2 L)
  8. customThe C6H14 was decanted off
  9. customthe residue chromatographed on silica gel
  10. washThe product was eluted with 2% CH3OH

출처 및 근거

ORD 기록
ord-ebf15d41f84e419a8d76a1acaf410486
출처 데이터셋
uspto-grants-1987_02
특허 번호
US04642311

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