Ethanol → Ethyl (2-aminoethyl)(methyl)phosphinate

HRID 1614912ノート

反応式

HRID 1614912 の反応式
[CH2:1]([O:3][P:4]([CH2:7][CH2:8][NH:9]C(OCC1C=CC=CC=1)=O)([CH3:6])=[O:5])[CH3:2].CCO>[Pd].CCOC(C)=O>[CH2:1]([O:3][P:4]([CH2:7][CH2:8][NH2:9])([CH3:6])=[O:5])[CH3:2]

参加物

5

反応物 2

HCID 702EthanolHCID 67033999(2-Benzyloxycarbonylamino-ethyl)-methyl-phosphinic acid ethyl ester

生成物 1

HCID 85676205Ethyl (2-aminoethyl)(methyl)phosphinate収率 90%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8857Ethyl Acetate溶媒

実験手順

(2-Benzyloxycarbonylamino-ethyl)-methyl-phosphinic acid ethyl ester (1.3 g, 4.56 mmol) and 10% Pd/C (485 mg) were combined in a flask and EtOH (46 mL) was added. The reaction flask atmosphere was exchanged for H2 and the reaction was run at room temperature until complete, as determined by TLC (eluent: 100% EtOAc). The reaction was then filtered through Supercell NF and the filtrate was concentrated to yield (2-amino-ethyl)-methyl-phosphinic acid ethyl ester (615 mg, 90%) as a yellow oil in which white crystals began to form under high vacuum.

後処理

  1. customwas run at room temperature
  2. filtrationThe reaction was then filtered through Supercell NF
  3. concentrationthe filtrate was concentrated

出典と根拠

ORDレコード
ord-8cd9e3c53e524f6ca27a6afb6d161606
出典データセット
uspto-grants-2014_07
特許番号
US08765722B2

反応ノート

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