Methyl butadienecarboxylate → HCID 20435989、化合物

HRID 1154034ノート

反応式

HRID 1154034 の反応式
[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]

参加物

5

反応物 3

HCID 73688Methyl butadienecarboxylateHCID 20435928HCID 20435928、化合物HCID 178418268HCID 178418268、化合物

生成物 1

HCID 20435989HCID 20435989、化合物収率 38.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

(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).

後処理

  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

出典と根拠

ORDレコード
ord-ded641e9cef2437dbf76b1aa9e60a607
出典データセット
uspto-grants-1984_12
特許番号
US04487929

反応ノート

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