Hydrochloric Acid → Methyl 6-chloro-5-hydroxynicotinate

HRID 709774노트

반응식

HRID 709774 반응식
[OH:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([CH:11]=1)[C:7]([O:9][CH3:10])=[O:8].[Cl:12][O-].[Na+].Cl>O>[Cl:12][C:3]1[C:2]([OH:1])=[CH:11][C:6]([C:7]([O:9][CH3:10])=[O:8])=[CH:5][N:4]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 354317Methyl 5-hydroxypyridine-3-carboxylateHCID 23665760Sodium Hypochlorite

생성물 1

HCID 46941479Methyl 6-chloro-5-hydroxynicotinate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a mixture of methyl 5-hydroxynicotinate (10.0 g) and water (2.0 mL) was added dropwise 5% aqueous sodium hypochlorite solution (69.2 mL) at 0° C., and the mixture was stirred for 2 hr. 2N Hydrochloric acid (50 mL) was added to the reaction mixture at 0° C., and the resulting white precipitate was collected by filtration. The crude crystals were washed with water, and the obtained solid was dissolved in acetonitrile. The solvent was evaporated under reduced pressure to give a crude product of the title compound (3.71 g) as a pale-yellow solid. This compound was used for the next step without further purification.

후처리

  1. filtrationthe resulting white precipitate was collected by filtration
  2. washThe crude crystals were washed with water
  3. dissolutionthe obtained solid was dissolved in acetonitrile
  4. customThe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-6a385d4fb3aa40f5942808a1da1785b2
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09181186B2

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