Hydrochloric Acid → 3,4-Dihydroxy-thiophene-2,5-dicarboxylic acid diethyl ester

HRID 984762

反応式

HRID 984762 の反応式
[C:1](OCC)(=[O:7])[C:2](OCC)=[O:3].[CH2:11]([O:13][C:14](=[O:21])[CH2:15][S:16][CH2:17][C:18]([O-:20])=[O:19])[CH3:12].O.Cl.[CH3:24][CH2:25]O>>[C:18]([C:17]1[S:16][C:15]([C:14]([O:13][CH2:11][CH3:12])=[O:21])=[C:1]([OH:7])[C:2]=1[OH:3])([O:20][CH2:24][CH3:25])=[O:19]

参加物

6

反応物 5

HCID 313Hydrochloric AcidHCID 702EthanolHCID 962WaterHCID 7268Diethyl OxalateHCID 86604148Thiobisacetate ethyl ester

生成物 1

HCID 2455033,4-Dihydroxy-thiophene-2,5-dicarboxylic acid diethyl ester

実験手順

Diethyl oxalate (6.58 g, 45 mmol) was added to 2,2′ thiobisacetate ethyl ester (4.66 g. 23 mmol) to produce a yellow-orange solution. A solution of Na (1.56 g, 68 mmol) in EtOH (24 mL) was added to produce a white/yellow precipitate, this was mixed well for 10 minutes. H2O (50 mL) was added to the reaction mass with cooling in an ice bath. Concentrated HCl was added dropwise until acidified. This was allowed to stand in the refrigerator for 12 days. At this point a cold filtration was done to isolate a white solid.

後処理

  1. customto produce a yellow-orange solution
  2. customto produce a white/yellow precipitate
  3. additionthis was mixed well for 10 minutes
  4. temperaturewith cooling in an ice bath
  5. filtrationAt this point a cold filtration
  6. customto isolate a white solid

出典と根拠

ORDレコード
ord-a39562d798354f8ca1166e4057d2ca2b
出典データセット
uspto-grants-2005_03
特許番号
US06869729B1

関連ノート

読み込み中…