Diethyl (benzylamino)methylphosphonate → Diethyl (aminomethyl)phosphonate

HRID 45644ノート

反応式

HRID 45644 の反応式
C([NH:8][CH2:9][P:10](=[O:17])([O:14][CH2:15][CH3:16])[O:11][CH2:12][CH3:13])C1C=CC=CC=1>C(O)C.C(O)(=O)C.[C].[Pd]>[NH2:8][CH2:9][P:10](=[O:17])([O:14][CH2:15][CH3:16])[O:11][CH2:12][CH3:13]

参加物

5

反応物 1

HCID 10923173Diethyl (benzylamino)methylphosphonate

生成物 1

HCID 1596920Diethyl (aminomethyl)phosphonate

試薬・触媒・溶媒 3

HCID 178418390HCID 178418390、化合物触媒HCID 176Acetic Acid溶媒HCID 702Ethanol溶媒

反応条件

温度
50 °C

実験手順

A 250-mL pressure tank reactor was purged, flushed and maintained with a hydrogen atmosphere, then, was added a solution of diethyl (benzylamino)methylphosphonate (3.5 g, 13.62 mmol, 1.00 equiv) in ethanol (180 mL), acetic acid (10 mL) and Palladium carbon (0.2 g, 0.10 equiv). The resulting solution was stirred for 24 h at 50° C. under 20 atm pressure. The solids were filtered out. The resulting mixture was concentrated under vacuum. This resulted in 2.0 g (crude) of the title compound as brown oil which was used without further purification.

後処理

  1. customA 250-mL pressure tank reactor was purged
  2. customflushed
  3. temperaturemaintained with a hydrogen atmosphere
  4. filtrationThe solids were filtered out
  5. concentrationThe resulting mixture was concentrated under vacuum

出典と根拠

ORDレコード
ord-4510b880f27d4920bce8c3650cf569ec
出典データセット
uspto-grants-2013_09
特許番号
US08541448B2

反応ノート

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