Potassium Hydroxide → Methyl 3-(N,N-dimethylaminothiocarbamoyloxy)pyridine-2-carboxylate

HRID 35545노트

반응식

HRID 35545 반응식
[OH:1][C:2]1[C:3]([C:8]([O:10][CH3:11])=[O:9])=[N:4][CH:5]=[CH:6][CH:7]=1.[OH-].[K+].[CH3:14][NH:15][N:16]([NH:20][CH3:21])[C:17](Cl)=[S:18]>O>[CH3:14][NH:15][N:16]([NH:20][CH3:21])[C:17]([O:1][C:2]1[C:3]([C:8]([O:10][CH3:11])=[O:9])=[N:4][CH:5]=[CH:6][CH:7]=1)=[S:18]

참가 물질

5

반응물 3

HCID 14797Potassium HydroxideHCID 819341Methyl 3-Hydroxy-2-pyridinecarboxylateHCID 86742401N,N-dimethylaminothiocarbamoyl chloride

생성물 1

HCID 86742400Methyl 3-(N,N-dimethylaminothiocarbamoyloxy)pyridine-2-carboxylate수율 75.8%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A solution of 3.06 g (20 mmol) of methyl 3-hydroxypyridine-2-carboxylate in 15 mL of water was made basic with 1.12 g KOH. To this solution was added 3.2 g (26 mmol) of N,N-dimethylaminothiocarbamoyl chloride and the solution was stirred at room temperature for 2 hours. The solution was partitioned between benzene and water and the aqueous layer was washed with two portions of water. The combined extracts were dried and concentrated to afford 4.1 g of a white solid, m.p. 74°-75° C.

후처리

  1. customThe solution was partitioned between benzene and water
  2. washthe aqueous layer was washed with two portions of water
  3. customThe combined extracts were dried
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-5b9c88c351b54a55b8f8e3550258e9d6
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04767766

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