Ethanol → HCID 178470113、化合物

HRID 599487ノート

反応式

HRID 599487 の反応式
[SH:1][C:2]1[S:3][CH:4]=[C:5]([C:7]([OH:9])=[O:8])[N:6]=1.OS(O)(=O)=O.[CH2:15](O)[CH3:16]>>[SH:1][C:2]1[S:3][CH:4]=[C:5]([C:7]([O:9][CH2:15][CH3:16])=[O:8])[N:6]=1

参加物

4

反応物 3

HCID 702EthanolHCID 1118Sulfuric AcidHCID 178524840HCID 178524840、化合物

生成物 1

HCID 178470113HCID 178470113、化合物

実験手順

To 2-mercaptothiazole-4-carboxylic acid (Ex. 19b, 4.2 g) in 50 mL ethyl alcohol was added 2 mL conc. H2SO4. The mixture was heated to reflux for 8 h and cooled. The solvent was removed under reduced pressure and the residue was poured onto 50 mL ice water. The solid was collected, washed with water and dried under vacuum. The crude product was recrystallized from 8 mL ethyl alcohol to afford ethyl 2-mercaptothiazole-4-carboxylate (2.3 g) as a yellow solid.

後処理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 8 h
  3. temperaturecooled
  4. customThe solvent was removed under reduced pressure
  5. additionthe residue was poured onto 50 mL ice water
  6. customThe solid was collected
  7. washwashed with water
  8. customdried under vacuum
  9. customThe crude product was recrystallized from 8 mL ethyl alcohol

出典と根拠

ORDレコード
ord-fb23ee1e14b8406a83273c164f96a2e1
出典データセット
uspto-grants-2011_03
特許番号
US07897776B2

反応ノート

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