Sodium Methoxide → 2-Piperidinone, 3-amino-3-(difluoromethyl)-

HRID 1648828ノート

反応式

HRID 1648828 の反応式
Cl.Cl.[F:3][CH:4]([F:15])[C:5]([NH2:14])([CH2:10][CH2:11][CH2:12][NH2:13])[C:6](OC)=[O:7].C[O-].[Na+]>CO>[NH2:14][C:5]1([CH:4]([F:15])[F:3])[CH2:10][CH2:11][CH2:12][NH:13][C:6]1=[O:7]

参加物

4

反応物 2

HCID 10942334Sodium MethoxideHCID 19966339HCID 19966339、化合物

生成物 1

HCID 5746312-Piperidinone, 3-amino-3-(difluoromethyl)-

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

To a solution of (±)-methyl 2-difluoromethyl-2,5-diaminopentanoate dihydrochloride (2.7 g) in dry methanol (30 ml) is added under nitrogen 2 equivalents of sodium methylate in methanol (0.46 g of sodium in 20 ml of methanol). The reaction mixture is stirred for 3 hours at room temperature, then the solvent is evaporated under reduced pressure. The residue is extracted with ether to yield crude (±)-3-amino-3-difluoromethyl-2-piperidone which is purified either by crystallization from CHCl3 /pentane (m.p. 149° C.) or by distillation (b.p. 135° C./0.05 mm Hg).

後処理

  1. customthe solvent is evaporated under reduced pressure
  2. extractionThe residue is extracted with ether

出典と根拠

ORDレコード
ord-2cd96121f06c43b5b1d8b871a127bb03
出典データセット
uspto-grants-1983_11
特許番号
US04413141

反応ノート

読み込み中…