Hydrochloric Acid → HCID 18441970、化合物

HRID 458447ノート

反応式

HRID 458447 の反応式
[N:1]1[C:6]([C:7]([O:9][CH2:10][CH3:11])=[O:8])=[CH:5][CH:4]=[C:3]([C:12]([O:14]CC)=[O:13])[N:2]=1.Cl>C(O)C.[OH-].[Na+].CCOCC>[CH2:10]([O:9][C:7]([C:6]1[N:1]=[N:2][C:3]([C:12]([OH:14])=[O:13])=[CH:4][CH:5]=1)=[O:8])[CH3:11]

参加物

6

反応物 2

HCID 313Hydrochloric AcidHCID 9815937HCID 9815937、化合物

生成物 1

HCID 18441970HCID 18441970、化合物

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒HCID 3283Diethyl Ether溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

To the diethyl 3,6-pyridazinedicarboxylate (5.0 g, 22.3 mmol) in 150 ml ethyl alcohol, 24.5 ml 1N NaOH was added. The mixture was stirred for 2 hours. The resulting salt was collected by filtration then was dissolved in minimum amount of water. The aqueous solution obtained was then acidified with 2N HCl in ether until the PH=2 and extracted with ethyl acetate. The combined extracts were washed with brine and dried over sodium sulfate. Removal of the solvent afforded 4.1 g of light yellowish oil. 1HNMR (400 MHz, CD3OD) δ 8.42 (s, 2H), 4.52 (q, 2H), 1.42 (t, 3H) ppm.

後処理

  1. filtrationThe resulting salt was collected by filtration
  2. dissolutionthen was dissolved in minimum amount of water
  3. customThe aqueous solution obtained
  4. extractionextracted with ethyl acetate
  5. washThe combined extracts were washed with brine
  6. dry with materialdried over sodium sulfate
  7. customRemoval of the solvent
  8. customafforded 4.1 g of light yellowish oil

出典と根拠

ORDレコード
ord-c84b8e4b32d3471e89a3ee32b61a6b33
出典データセット
uspto-grants-2007_03
特許番号
US07189851B2

反応ノート

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