3-Mercaptopropionic Acid → HCID 178482013、化合物

HRID 35264

反応式

HRID 35264 の反応式
[SH:1][CH2:2][CH2:3][C:4](O)=O.[CH3:7][N:8]1[C:12]([CH2:13]Cl)=[N:11][N:10]=[N:9]1.[OH-:15].[Na+]>CC(C)=O>[CH3:7][N:8]1[C:12]([CH2:13][CH2:4][CH2:3][C:2]([OH:15])=[S:1])=[N:11][N:10]=[N:9]1

参加物

5

反応物 3

HCID 65143-Mercaptopropionic AcidHCID 14798Sodium HydroxideHCID 122050865-(chloromethyl)-1-methyl-1H-1,2,3,4-tetrazole

生成物 1

HCID 178482013HCID 178482013、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

3-Mercaptopropionic acid (1.6 g) is dissolved in 1N aqueous sodium hydroxide solution (45 ml) and thereto is added dropwise a solution of 1-methyl-5-chloromethyl-1,2,3,4-tetrazole (15.2 g) in acetone (20 ml) with stirring under ice-cooling. Stirring is continued for 3 hours under ice-cooling. Acetone is distilled off and the residue is acidified with concentrated hydrochloric acid, saturated with sodium chloride and then, extracted with chloroform. The chloroform solution is dried over magnesium sulfate. After chloroform is distilled off, the residue is subjected to column chromatography (Kieselgel 60, made by Merck) by eluting the column with chloroform-methanol (10:1, V/V) to give 3-(1-methyl-1,2,3,4-tetrazol-5-yl)methylthio-propionic acid (2.1 g) as a colorless liquid.

後処理

  1. temperaturecooling
  2. stirringStirring
  3. temperaturecooling
  4. distillationAcetone is distilled off
  5. extractionextracted with chloroform
  6. dry with materialThe chloroform solution is dried over magnesium sulfate
  7. distillationAfter chloroform is distilled off
  8. washby eluting the column with chloroform-methanol (10:1, V/V)

出典と根拠

ORDレコード
ord-100212a40e3c4fc68a027c2e9a8bc3e9
出典データセット
uspto-grants-1988_08
特許番号
US04766120

関連ノート

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