HCID 86637890, 화합물 → ethyl (4-hydroxy-2-methyl-1H-benzimidazol-1-yl)acetate

HRID 2389349노트

반응식

HRID 2389349 반응식
C([O:8][C:9]1[C:17]2[N:16]=[C:15]([CH3:18])[N:14]([CH2:19][C:20]([O:22][CH2:23][CH3:24])=[O:21])[C:13]=2[CH:12]=[CH:11][CH:10]=1)C1C=CC=CC=1.[H][H]>CCO.C1COCC1.[Pd]>[OH:8][C:9]1[C:17]2[N:16]=[C:15]([CH3:18])[N:14]([CH2:19][C:20]([O:22][CH2:23][CH3:24])=[O:21])[C:13]=2[CH:12]=[CH:11][CH:10]=1

참가 물질

6

반응물 2

HCID 86637890HCID 86637890, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 86637909ethyl (4-hydroxy-2-methyl-1H-benzimidazol-1-yl)acetate수율 93.2%

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 702Ethanol용매HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of ethyl [4-(benzyloxy)-2-methyl-1H-benzimidazol-1-yl]acetate (2.57 g) in a mixture of EtOH (25.7 mL) and THF (12.9 mL) was added 10% palladium on carbon (50% wet, 0.78 g) at ambient temperature, and the resultant mixture was hydrogenated under atmospheric pressure of hydrogen for 2 hours. The catalyst was removed by filtration and evaporated in vacuo to give crude solid. The crude solid was recrystallized from solvent (EtOAc:n-hexane) to give ethyl (4-hydroxy-2-methyl-1H-benzimidazol-1-yl)acetate (1.73 g) as a white solid.

후처리

  1. customThe catalyst was removed by filtration
  2. customevaporated in vacuo
  3. customto give crude solid
  4. customThe crude solid was recrystallized from solvent (EtOAc:n-hexane)

출처 및 근거

ORD 기록
ord-6b8cfe2297b444ab816c52ba34203cd1
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08273745B2

반응 노트

불러오는 중…