Ethanol → HCID 178470503、化合物

HRID 872919ノート

反応式

HRID 872919 の反応式
CCOC([CH2:6][CH2:7][C:8]([C:10]([O:12][CH2:13][CH3:14])=[O:11])=O)=O.Cl.Cl.[NH2:17][NH2:18].[OH2:19].[C:20]([O-])(O)=O.[Na+].[CH2:25](O)[CH3:26]>>[CH2:25]([O:19][C:20]1[NH:18][N:17]=[C:8]([C:10]([O:12][CH2:13][CH3:14])=[O:11])[C:7]=1[CH3:6])[CH3:26]

参加物

6

反応物 5

HCID 702EthanolHCID 962WaterHCID 17548Hydrazine, dihydrochlorideHCID 800701,5-Diethyl 2-oxopentanedioateHCID 516892Sodium Bicarbonate

生成物 1

HCID 178470503HCID 178470503、化合物収率 80%

実験手順

A solution of diethyl oxalpropionate (9.15 ml, 49.5 mmol) and hydrazine dihydrochloride (6.23 g, 59.3 mmol) in ethanol (50 ml) was refluxed for 1 h. The mixture was then cooled and water (150 ml) was added. The solution was neutralised with solid NaHCO3 and extracted four times with EtOAc. The organic phase was washed with brine and water, dried with Na2SO4 and evaporated to dryness affording 7.81 g (80%) of the title compound. LC-MS: [M+1]=199.22.

後処理

  1. temperatureThe mixture was then cooled
  2. extractionextracted four times with EtOAc
  3. washThe organic phase was washed with brine and water
  4. dry with materialdried with Na2SO4
  5. customevaporated to dryness

出典と根拠

ORDレコード
ord-ff515dbe94454f91bfb10d0602cd17dc
出典データセット
uspto-grants-2015_03
特許番号
US08975254B2

反応ノート

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