Methyl butadienecarboxylate → HCID 20435989, 화합물

HRID 1154034노트

반응식

HRID 1154034 반응식
[CH3:1][C:2]1([CH2:9][CH2:10][O:11][CH:12]2[CH2:17][CH2:16][CH2:15][CH2:14][O:13]2)[C:6](=[O:7])[NH:5][NH:4][C:3]1=[O:8].[C:18]([O:24][CH3:25])(=[O:23])[CH:19]=[CH:20][CH:21]=[CH2:22].C([O-])(=O)C.C([O-])(=O)C.C([O-])(=O)C.C([O-])(=O)C.[Pb+4]>ClCCl>[CH3:1][C:2]1([CH2:9][CH2:10][O:11][CH:12]2[CH2:17][CH2:16][CH2:15][CH2:14][O:13]2)[C:6](=[O:7])[N:5]2[CH2:22][CH:21]=[CH:20][CH:19]([C:18]([O:24][CH3:25])=[O:23])[N:4]2[C:3]1=[O:8]

참가 물질

5

반응물 3

HCID 73688Methyl butadienecarboxylateHCID 20435928HCID 20435928, 화합물HCID 178418268HCID 178418268, 화합물

생성물 1

HCID 20435989HCID 20435989, 화합물수율 38.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

(B)(b) A mixture of 14.52 g (0.06 mol) of 4-methyl-4-[2-(tetrahydro-2-pyranyloxy)ethyl]pyrazolidine-3,5-dione and 6.72 g (0.066 mol) of methyl penta-2,4-dienoate in 150 ml of dry dichloromethane was stirred at room temperature under a stream of nitrogen. A solution of 26.64 g (0.06 mol) of lead tetraacetate in 100 ml of dry dichloromethane was added dropwise, the blue color being allowed to fade between additions. When the addition was complete and no blue color persisted, the resulting suspension was filtered. The filtrate was washed with saturated aqueous sodium bicarbonate, dried over magnesium sulfate and evaporated to give 8.12 g (38%) of methyl 2,3,5,8-tetrahydro-2-methyl-1,3-dioxo-2-[2-(tetrahydro-2-pyranyloxy)ethyl]-1H-pyrazolo[1,2-a]pyridazine-5-carboxylate having a melting point of 126.5°-127.6° C. (from diethyl ether).

후처리

  1. additionWhen the addition
  2. filtrationthe resulting suspension was filtered
  3. washThe filtrate was washed with saturated aqueous sodium bicarbonate
  4. dry with materialdried over magnesium sulfate
  5. customevaporated

출처 및 근거

ORD 기록
ord-ded641e9cef2437dbf76b1aa9e60a607
출처 데이터셋
uspto-grants-1984_12
특허 번호
US04487929

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