Hydrazine hydrate (1:1) → Ammonia

HRID 20271

反応式

HRID 20271 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[N:3][C:2]=1[O:7][CH2:8][C:9]([O:11]CC)=O.O.[NH2:15][NH2:16]>C(O)(C)C>[NH3:1].[N:1]1[CH:6]=[CH:5][CH:4]=[N:3][C:2]=1[O:7][CH2:8][C:9]([NH:15][NH2:16])=[O:11]

参加物

5

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 22396258Ethyl 2-pyrimidinyloxyacetate

生成物 2

HCID 222AmmoniaHCID 593475352-(Pyrimidin-2-yloxy)acetohydrazide

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

A mixture of ethyl 2-pyrimidinyloxyacetate (GB2373186, step i ex 368) (4.4 g, 24.15 mmol) and hydrazine hydrate (5 mL, 160 mmol) in isopropanol (30 mL) was heated under reflux for 1 hour. The mixture was then cooled and concentrated under reduced pressure and the residue was purified by column chromatography on silica gel using dichloromethane:methanol:0.88 ammonia (100:0:0 to 100:10:1) to provide the title compound, 600 mg.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 1 hour
  3. temperatureThe mixture was then cooled
  4. concentrationconcentrated under reduced pressure
  5. customthe residue was purified by column chromatography on silica gel

出典と根拠

ORDレコード
ord-acc3963df842493485c6c9e822535ce0
出典データセット
uspto-grants-2010_06
特許番号
US07745630B2

関連ノート

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