Ammonia → 2-Amino-4-methylpyridine-3-carbonitrile

HRID 233589ノート

反応式

HRID 233589 の反応式
[C:1]([C:3]([C:11]#[N:12])=[CH:4][C:5]([CH3:10])=COCC)#[N:2].[C:13](C(C#N)=CC(C)C(OCC)OCC)#N.[NH3:28]>>[NH2:28][C:11]1[C:3]([C:1]#[N:2])=[C:4]([CH3:13])[CH:5]=[CH:10][N:12]=1

参加物

4

反応物 3

HCID 222AmmoniaHCID 197072091,1-Dicyano-4,4-diethoxy-3-methyl-1-buteneHCID 542610241,1-Dicyano-4-ethoxy-3-methyl-1,3-butadiene

生成物 1

HCID 103968872-Amino-4-methylpyridine-3-carbonitrile

実験手順

A solution of about 6.1 grams (0.038 mole) of a mixture of 1,1-dicyano-4-ethoxy-3-methyl-1,3-butadiene and 1,1-dicyano-4,4-diethoxy-3-methyl-1-butene in 200 mL of saturated methanolic ammonia is stirred at ambient temperature for about 15 hours. After this time the solvent is removed under reduced pressure, and the residue is partitioned between 160 mL of aqueous 1N hydrochloric acid and 160 mL of ethyl acetate. The aqueous layer is separated and poured into 160 mL of an aqueous solution saturated with sodium bicarbonate. The resultant solid is collected by filtration and dried, yielding about 2.6 grams of 2-amino-3-cyano-4-methylpyridine. Steps A and B are repeated.

後処理

  1. customAfter this time the solvent is removed under reduced pressure
  2. customthe residue is partitioned between 160 mL of aqueous 1N hydrochloric acid and 160 mL of ethyl acetate
  3. customThe aqueous layer is separated
  4. additionpoured into 160 mL of an aqueous solution saturated with sodium bicarbonate
  5. filtrationThe resultant solid is collected by filtration
  6. customdried

出典と根拠

ORDレコード
ord-cab2cceda4484f56bccd489b4a522de9
出典データセット
uspto-grants-1997_01
特許番号
US05593998

反応ノート

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