Hydrochloric Acid → HCID 19096301、化合物

HRID 486717ノート

反応式

HRID 486717 の反応式
[CH2:1]([O:3][C:4]([CH:6]1[CH2:10][CH2:9][CH:8]([C:11]([O:13]CC)=[O:12])[S:7]1)=[O:5])[CH3:2].[OH-].[K+].C(OCC)C.Cl>C(O)C.O>[C:11]([CH:8]1[CH2:9][CH2:10][CH:6]([C:4]([O:3][CH2:1][CH3:2])=[O:5])[S:7]1)([OH:13])=[O:12]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 14797Potassium HydroxideHCID 14993186HCID 14993186、化合物

生成物 1

HCID 19096301HCID 19096301、化合物収率 78%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒2 回HCID 962Water溶媒

実験手順

To a solution of 2,5-diethoxycarbonyltetrahydrothiophene (2.4 g) in ethanol (10 ml), potassium hydroxide (0.64 g) dissolved in ethanol (10 ml) was added dropwise and the mixture was stirred for 1 hour at room temperature. To the reaction mixture, diethyl ether and water were added. Aqueous layer was acidified with 2N hydrochloric acid and extracted with ethyl acetate. The organic layer was washed with saturated sodium chloride solution, dried over anhydrous sodium sulfate and concentrated in vacuo to give 1.6 g (78%) of 2-carboxy-5-ethoxycarbonyltetrahydrothiophene.

後処理

  1. additionwas added dropwise
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with saturated sodium chloride solution
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-6c17c3e197b14e76bff124ed188d0b42
出典データセット
uspto-grants-1994_03
特許番号
US05292767

反応ノート

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