HCID 10961905、化合物 → Tetraethyl aminomethylenediphosphonate

HRID 487050ノート

反応式

HRID 487050 の反応式
C([N:8]([CH:16]([P:25]([O:30][CH2:31][CH3:32])(=[O:29])[O:26][CH2:27][CH3:28])[P:17]([O:22][CH2:23][CH3:24])(=[O:21])[O:18][CH2:19][CH3:20])CC1C=CC=CC=1)C1C=CC=CC=1>C(O)C.[Pd]>[NH2:8][CH:16]([P:17]([O:22][CH2:23][CH3:24])(=[O:21])[O:18][CH2:19][CH3:20])[P:25]([O:26][CH2:27][CH3:28])(=[O:29])[O:30][CH2:31][CH3:32]

参加物

4

反応物 1

HCID 10961905HCID 10961905、化合物

生成物 1

HCID 2773808Tetraethyl aminomethylenediphosphonate

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

17.1 g (35.4 mmol) of tetraethyl N,N-dibenzyl-aminomethane-1,1-bisphosphonate are dissolved in 170 ml of ethanol and 3.4 g of 5% strength Pd/C are added. Hydrogenation is carried out at normal pressure. After absorption of 100 ml of hydrogen, a further 3.4 g of 5% strength Pd/C are added and the hydrogenation is completed at normal pressure and room temperature (reaction time about 16 hours). The catalyst is then filtered off with suction. After removal of the solvent, 10.9 g of crude product are obtained. This is purified on a silica gel column using ethanol as the eluent.

後処理

  1. customAfter absorption of 100 ml of hydrogen
  2. additiona further 3.4 g of 5% strength Pd/C are added
  3. customthe hydrogenation is completed at normal pressure and room temperature (reaction time about 16 hours)
  4. filtrationThe catalyst is then filtered off with suction
  5. customAfter removal of the solvent, 10.9 g of crude product
  6. customare obtained
  7. customThis is purified on a silica gel column

出典と根拠

ORDレコード
ord-c04f4f2ab1214434962a49c8b3fa8f7a
出典データセット
uspto-grants-1994_03
特許番号
US05294608

反応ノート

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