Hydrochloric Acid → HCID 18441970, 화합물

HRID 458447노트

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HRID 458447 반응식
[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]

참가 물질

6

반응물 2

HCID 313Hydrochloric AcidHCID 9815937HCID 9815937, 화합물

생성물 1

HCID 18441970HCID 18441970, 화합물

시약·촉매·용매 3

HCID 702Ethanol용매HCID 3283Diethyl Ether용매HCID 14798Sodium Hydroxide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c84b8e4b32d3471e89a3ee32b61a6b33
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07189851B2

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