Sulfuric Acid → Cyclopenta[c]thiophene-4,6-dione

HRID 868780

反応式

HRID 868780 の反応式
[S:1]1[CH:5]=[C:4]([C:6]([O:8]CC)=O)[C:3]([C:11]([O:13]CC)=O)=[CH:2]1.[O-][CH2:17]C.[Na+].C(OCC)(=O)C.S(=O)(=O)(O)O>O>[CH:5]1[S:1][CH:2]=[C:3]2[C:11](=[O:13])[CH2:17][C:6](=[O:8])[C:4]=12

参加物

6

反応物 4

HCID 1118Sulfuric AcidHCID 8857Ethyl AcetateHCID 2723922Sodium ethoxideHCID 12197673Diethyl thiophene-3,4-dicarboxylate

生成物 1

HCID 399283Cyclopenta[c]thiophene-4,6-dione

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

In a dry 3-neck flask with an argon inlet and a water condenser, diethyl thiophene-3,4-dicarboxylate (3.7 g, 16.2 mmol) is mixed with sodium ethoxide (1.1 g, 16.2 mmol). After heating to 100° C. ethyl acetate (1.4 g, 16.2 mmol) is added through syringe pump over one hour. The mixture was further heated for a few hours. The residue was redissolved in water at 70° C. and concentrated sulfuric acid is added (1 mL). The mixture is heated at this temperature for one hour to ensure complete decarboxylation.

後処理

  1. additionis added through syringe pump over one hour
  2. temperatureThe mixture was further heated for a few hours
  3. temperatureThe mixture is heated at this temperature for one hour

出典と根拠

ORDレコード
ord-2b6180bbf40a429c873ccf89181867b6
出典データセット
uspto-grants-2015_03
特許番号
US08968885B2

関連ノート

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