Dimethyl acetylenedicarboxylate → HCID 12437416, 화합물

HRID 1448678노트

반응식

HRID 1448678 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 was 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-a0897120cf9542af9a82bebdd8e5cc24
출처 데이터셋
uspto-grants-1980_02
특허 번호
US04187099

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