Dimethyl acetylenedicarboxylate → HCID 12437416、化合物

HRID 614176ノート

反応式

HRID 614176 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 12437416HCID 12437416、化合物収率 25.2%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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°.

後処理

  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)

出典と根拠

ORDレコード
ord-115c8ba374934855809c26cc0094f63f
出典データセット
uspto-grants-1979_03
特許番号
US04144047

反応ノート

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