Dimethyl acetylenedicarboxylate → HCID 12437416, 화합물

HRID 614176노트

반응식

HRID 614176 반응식
[C:1]([C:7]([O:9][CH3:10])=[O:8])#[C:2][C:3]([O:5][CH3:6])=[O:4].[N+:11]([C:14]1[CH:19]=[CH:18][C:17]([C:20]2OC(=O)[S:22][N:21]=2)=[CH:16][CH:15]=1)([O-:13])=[O:12]>C(OCC)(=O)C>[N+:11]([C:14]1[CH:15]=[CH:16][C:17]([C:20]2[C:2]([C:3]([O:5][CH3:6])=[O:4])=[C:1]([C:7]([O:9][CH3:10])=[O:8])[S:22][N:21]=2)=[CH:18][CH:19]=1)([O-:13])=[O:12]

참가 물질

4

반응물 2

HCID 12980Dimethyl acetylenedicarboxylateHCID 12437399(4-Nitrophenyl)-1,3,4-oxathiazol-2-one

생성물 1

HCID 12437416HCID 12437416, 화합물수율 25.2%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

Dimethyl acetylenedicarboxylate (85.26 g, 0.6 mol) and 5-(p-nitrophenyl)-1,3,4-oxathiazol-2-one (33.63 g, 0.15 mol) were heated as given above for 15 hours. Crystallization of the brown solid from methanol (2X) gave little improvement in purity. The brown solid as decolorized in ethyl acetate solution and recrystallized (3X) to give 12.2 g (0.0378 mol, 25.2%) of dark gold solid, m.p. 142°-143°.

후처리

  1. customas given above for 15 hours
  2. customCrystallization of the brown solid from methanol (2X)
  3. customgave little improvement in purity
  4. customrecrystallized (3X)

출처 및 근거

ORD 기록
ord-115c8ba374934855809c26cc0094f63f
출처 데이터셋
uspto-grants-1979_03
특허 번호
US04144047

반응 노트

불러오는 중…