Hydrazine hydrate (1:1) → 6-Methylpicolinimidohydrazide

HRID 1851243ノート

反応式

HRID 1851243 の反応式
[CH3:1][C:2]1[N:7]=[C:6]([C:8]#[N:9])[CH:5]=[CH:4][CH:3]=1.O.[NH2:11][NH2:12]>C(O)C>[CH3:1][C:2]1[N:7]=[C:6]([C:8](=[N:11][NH2:12])[NH2:9])[CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 741826-Methylpyridine-2-carbonitrile

生成物 1

HCID 573576606-Methylpicolinimidohydrazide収率 78.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

11.97 g (101.4 mmol) 6-methylpyridine-2-carbonitrile are dissolved in 25 mL ethanol. After addition of 36.3 mL (304.05 mmol) hydrazine hydrate (w=30%) the reaction mixture is stirred for 24 hours at room temperature. The precipitated product (K1=1.45 g) has been filtered off and the filtrate is evaporated to ⅓ of its volume. After dilution with water the reaction mixture is extracted three times with ethyl acetate. The combined organic extracts are washed with brine and dried (Na2SO4). The solvent has been removed yielding a K2 (11.11 g) of the desired product. The overall yield is 78.9%.

後処理

  1. filtrationThe precipitated product (K1=1.45 g) has been filtered off
  2. customthe filtrate is evaporated
  3. extractionAfter dilution with water the reaction mixture is extracted three times with ethyl acetate
  4. washThe combined organic extracts are washed with brine
  5. dry with materialdried (Na2SO4)
  6. customThe solvent has been removed

出典と根拠

ORDレコード
ord-f60331f5ef99493cb92f950da32f6571
出典データセット
uspto-grants-2015_02
特許番号
US08957064B2

反応ノート

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