Ethyl 4-diethoxyphosphoryl-3-oxobutanoate → HCID 54162917、化合物

HRID 2226660ノート

反応式

HRID 2226660 の反応式
[CH2:1]([O:3][P:4]([O:15][CH2:16][CH3:17])([CH2:6][C:7](=[O:14])[CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10])=[O:5])[CH3:2]>CO.O=[Pt]=O>[CH2:12]([O:11][C:9](=[O:10])[CH2:8][CH:7]([OH:14])[CH2:6][P:4]([O:3][CH2:1][CH3:2])([O:15][CH2:16][CH3:17])=[O:5])[CH3:13]

参加物

4

反応物 1

HCID 11129233Ethyl 4-diethoxyphosphoryl-3-oxobutanoate

生成物 1

HCID 54162917HCID 54162917、化合物収率 101.1%

試薬・触媒・溶媒 2

HCID 345198Adams' catalyst触媒HCID 887Methanol溶媒

実験手順

The title compound of Example 7 (17 g, 63.8 mmol) was dissolved in 200 mL of methanol. To this solution was added PtO2 (1.7 g, 10% w/w). The mixture was degassed by evacuation of air, then refilling with hydrogen. This degassing procedure was repeated three times. The pressure in the Parr-shaker was set to 50 psi, and the mixture was shaken for 36 hours. The catalyst was filtered through a Celite pad and the filtrate was concentrated on a rotavap to give 17.3 g (~100%) of the title compound as a white solid, m.p. 33° C. to 35° C.

後処理

  1. customThe mixture was degassed by evacuation of air
  2. filtrationThe catalyst was filtered through a Celite pad
  3. concentrationthe filtrate was concentrated on a rotavap

出典と根拠

ORDレコード
ord-33eb8ac340884b83b070adcad0e00683
出典データセット
uspto-grants-1994_09
特許番号
US05349069

反応ノート

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