Hydrochloric Acid → 2-Methoxy-6-(2-oxopyrrolidin-1-yl)pyridine-4-carboxylic acid

HRID 1612469노트

반응식

HRID 1612469 반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([C:9]([O:11]C(C)(C)C)=[O:10])[CH:6]=[C:5]([N:16]2[CH2:20][CH2:19][CH2:18][C:17]2=[O:21])[N:4]=1.Cl>O1CCOCC1>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([C:9]([OH:11])=[O:10])[CH:6]=[C:5]([N:16]2[CH2:20][CH2:19][CH2:18][C:17]2=[O:21])[N:4]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 22252983t-Butyl 2-methoxy-6-(2-oxopyrrolidin-1-yl)pyridine-4-carboxylate

생성물 1

HCID 222530372-Methoxy-6-(2-oxopyrrolidin-1-yl)pyridine-4-carboxylic acid

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

t-Butyl 2-methoxy-6-(2-oxopyrrolidin-1-yl)pyridine-4-carboxylate (D57) (0.27 g) was stirred overnight in a dioxan solution of HCl (4M; 10 mL). The solution was evaporated to dryness and dissolved in sat. aq. sodium bicarbonate. The basic aqueous solution was washed twice with ether and was then acidified to pH4 with citric acid solution (10% aq.), saturated with NaCl and extracted three times with ethyl acetate. The combined extracts were washed with brine, dried and evaporated to a solid which was triturated with water, collected by filtration and dried at 50° C. in vacuo (silica gel desiccant). The title compound (D58) was obtained as an off-white solid (0.141 g).

후처리

  1. customThe solution was evaporated to dryness
  2. dissolutiondissolved in sat. aq. sodium bicarbonate
  3. washThe basic aqueous solution was washed twice with ether
  4. extractionextracted three times with ethyl acetate
  5. washThe combined extracts were washed with brine
  6. customdried
  7. customevaporated to a solid which
  8. customwas triturated with water
  9. filtrationcollected by filtration
  10. customdried at 50° C. in vacuo (silica gel desiccant)

출처 및 근거

ORD 기록
ord-aecc84ac612b42df8ca01712cd73b4cb
출처 데이터셋
uspto-grants-2006_01
특허 번호
US06992103B2

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