Lithium hydroxide, monohydrate → 5H-[1,3]dioxolo[4,5-f]indole-6-carboxylic acid

HRID 62653노트

반응식

HRID 62653 반응식
[O:1]1[C:5]2=[CH:6][C:7]3[CH:8]=[C:9]([C:13]([O:15]CC)=[O:14])[NH:10][C:11]=3[CH:12]=[C:4]2[O:3][CH2:2]1.O[Li].O>C(O)C>[O:1]1[C:5]2=[CH:6][C:7]3[CH:8]=[C:9]([C:13]([OH:15])=[O:14])[NH:10][C:11]=3[CH:12]=[C:4]2[O:3][CH2:2]1

참가 물질

4

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 10513792Ethyl 5H-[1,3]dioxolo[4,5-f]indole-6-carboxylate

생성물 1

HCID 9073915H-[1,3]dioxolo[4,5-f]indole-6-carboxylic acid수율 86%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of ethyl 5H-[1,3]dioxolo[4,5-f]indole-6-carboxylate (I-4b: 0.4 g, 1.716 mmol) in ethanol (8 mL) was added LiOH.H2O (0.144 g, 3.433 mmol) and refluxed for 16 h. The solvent was evaporated under reduced pressure and the residue was dissolved in water (10 mL). The aqueous layer was acidified with 10% aq. HCl solution to pH 6.0, precipitated solid was filtered, residue was washed with water and dried under vacuum to afford 0.3 g (86%) of 5H-[1,3]dioxolo[4,5-f]indole-6-carboxylic acid (I-4c) as an off-white solid.

후처리

  1. temperaturerefluxed for 16 h
  2. customThe solvent was evaporated under reduced pressure
  3. dissolutionthe residue was dissolved in water (10 mL)
  4. customprecipitated solid
  5. filtrationwas filtered
  6. washresidue was washed with water
  7. customdried under vacuum

출처 및 근거

ORD 기록
ord-f21ed9fa3d754708bfa80aee6037189b
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09447039B2

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