3-Mercaptopropionic Acid → HCID 178482013, 화합물

HRID 35264

반응식

HRID 35264 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 178482013HCID 178482013, 화합물

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-100212a40e3c4fc68a027c2e9a8bc3e9
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04766120

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