Methanol → Methyl 6-amino-5-nitropyridine-3-carboxylate

HRID 427497ノート

反応式

HRID 427497 の反応式
Cl[C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][C:5]([C:6](Cl)=[O:7])=[CH:4][N:3]=1.[OH-:14].[NH4+:15].[CH3:16]O>>[NH2:15][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][C:5]([C:6]([O:14][CH3:16])=[O:7])=[CH:4][N:3]=1

参加物

4

反応物 3

HCID 887MethanolHCID 14923Ammonium HydroxideHCID 113680196-Chloro-5-nitronicotinoyl chloride

生成物 1

HCID 13768248Methyl 6-amino-5-nitropyridine-3-carboxylate収率 45.9%

実験手順

6-Chloro-5-nitronicotinoyl chloride (22.0 g, 0.1 mol) was cooled to +5° C. Methanol was added dropwise during 30 min and the reaction mixture was stirred for 60 min. The temperature was not allowed to raise over +10° C. Ammonium hydroxide (25%, 400 ml) was added dropwise to the reaction mixture and the mixture was stirred at room temperature for 20 h. The product was filtered off, washed with water and dried to give 9.0 g (45.9%) of the title compound.

後処理

  1. temperatureto raise over +10° C
  2. stirringthe mixture was stirred at room temperature for 20 h
  3. filtrationThe product was filtered off
  4. washwashed with water
  5. customdried

出典と根拠

ORDレコード
ord-b8961e0ca40d41a384984305b55b3e15
出典データセット
uspto-grants-2001_11
特許番号
US06313137B1

反応ノート

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