Hydrochloric Acid → methyl 1H-1,3-benzodiazole-5-carboxylate

HRID 1419122

반응식

HRID 1419122 반응식
[N:1]1[C:5]2[CH:6]=[CH:7][C:8]([C:10]([OH:12])=[O:11])=[CH:9][C:4]=2[NH:3][CH:2]=1.[CH3:13]O.Cl>O1CCOCC1>[N:1]1[C:5]2[CH:6]=[CH:7][C:8]([C:10]([O:12][CH3:13])=[O:11])=[CH:9][C:4]=2[NH:3][CH:2]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 4594565-Benzimidazolecarboxylic acid

생성물 1

HCID 2779733methyl 1H-1,3-benzodiazole-5-carboxylate

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A mixture of 10 g of 5-benzimidazolecarboxylic acid, 150 ml of methanol and 100 ml of a 4N solution of hydrogen chloride in 1,4-dioxane was agitated ultrasonically for 4 hours. At the end of this time, the solvent was removed by distillation under reduced pressure, after which 300 ml of methanol and 3.5 g of lithium borohydride were added to the residue and the mixture was stirred for 1 hour. The solvent was then removed by evaporation under reduced pressure and the residue was mixed with an aqueous solution of sodium chloride, after which it was extracted with ethyl acetate. The solvent was removed by distillation under reduced pressure, to give 5.44 g of the title compound, melting at 136°-138° C.

후처리

  1. customAt the end of this time, the solvent was removed by distillation under reduced pressure
  2. additionafter which 300 ml of methanol and 3.5 g of lithium borohydride were added to the residue
  3. stirringthe mixture was stirred for 1 hour
  4. customThe solvent was then removed by evaporation under reduced pressure
  5. additionthe residue was mixed with an aqueous solution of sodium chloride
  6. extractionafter which it was extracted with ethyl acetate
  7. customThe solvent was removed by distillation under reduced pressure

출처 및 근거

ORD 기록
ord-c11418e650954deeae25fbb9abf65142
출처 데이터셋
uspto-grants-1999_03
특허 번호
US05886014

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