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

HRID 35545

反応式

HRID 35545 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5b9c88c351b54a55b8f8e3550258e9d6
出典データセット
uspto-grants-1988_08
特許番号
US04767766

関連ノート

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