Acetic Acid → HCID 178523102、化合物

HRID 2072677

反応式

HRID 2072677 の反応式
[Na].[C:2]([NH2:8])(=[O:7])[CH2:3][C:4]([NH2:6])=[O:5].C(O[C:12](=O)[CH2:13][NH:14][C:15](=[O:21])[C:16]1[S:20][CH:19]=[CH:18][CH:17]=1)C.C(O)(=O)C>C(O)C.O>[C:16]1([C:15]([NH:14][CH2:13][C:12]2[N:6]=[C:4]([OH:5])[CH:3]=[C:2]([OH:7])[N:8]=2)=[O:21])[S:20][CH:19]=[CH:18][CH:17]=1

参加物

7

反応物 4

HCID 176Acetic AcidHCID 7911MalonamideHCID 1720748Ethyl N-(thiophene-2-carbonyl)glycinateHCID 5360545Sodium

生成物 1

HCID 178523102HCID 178523102、化合物収率 29.9%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

反応条件

温度
60 °C

実験手順

To a solution of sodium (1.4 g) in ethanol (120 ml) was added malonamide (3.8 g) and the mixture was heated at 60° C. for an hour under stirring. Then after added N-(2-thenoyl)glycine ethyl ester (8 g), the mixture was refluxed for 6 hours. The mixture was concentrated to give the residue which was diluted with water. The aqueous mixture was neutralized by adding acetic acid to deposit a crystalline product which was collected by filtration and recrystallized from dimethylformamide (DMF) to give the objective product (2.8 g) as colorless crystals, mp 270°-275° C. (decompd.).

後処理

  1. temperaturethe mixture was refluxed for 6 hours
  2. concentrationThe mixture was concentrated
  3. customto give the residue which
  4. filtrationwas collected by filtration
  5. customrecrystallized from dimethylformamide (DMF)

出典と根拠

ORDレコード
ord-55e0a80065a640df8af85270c226556e
出典データセット
uspto-grants-1990_04
特許番号
US04914104

関連ノート

読み込み中…