Hydrazine hydrate (1:1) → 6-Methylpicolinimidohydrazide

HRID 1851243노트

반응식

HRID 1851243 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 573576606-Methylpicolinimidohydrazide수율 78.9%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-f60331f5ef99493cb92f950da32f6571
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08957064B2

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