HCID 10961905, 화합물 → Tetraethyl aminomethylenediphosphonate

HRID 487050노트

반응식

HRID 487050 반응식
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]

참가 물질

4

반응물 1

HCID 10961905HCID 10961905, 화합물

생성물 1

HCID 2773808Tetraethyl aminomethylenediphosphonate

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c04f4f2ab1214434962a49c8b3fa8f7a
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05294608

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