4-Methylmorpholine → 1,4-Bis(tert-butoxycarbonyl)-2-formylmethylpiperazine

HRID 352831ノート

反応式

HRID 352831 の反応式
CN1CCOCC1.[C:8]([O:12][C:13]([N:15]1[CH2:20][CH2:19][N:18]([C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22])[CH2:17][CH:16]1[CH2:28][CH2:29][OH:30])=[O:14])([CH3:11])([CH3:10])[CH3:9]>C(Cl)Cl.[Ru]([O-])(=O)(=O)=O.C([N+](CCC)(CCC)CCC)CC>[C:8]([O:12][C:13]([N:15]1[CH2:20][CH2:19][N:18]([C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22])[CH2:17][CH:16]1[CH2:28][CH:29]=[O:30])=[O:14])([CH3:11])([CH3:10])[CH3:9]

参加物

5

反応物 2

HCID 79724-MethylmorpholineHCID 22710988di-tert-Butyl 2-(2-hydroxyethyl)piperazine-1,4-dicarboxylate

生成物 1

HCID 227100181,4-Bis(tert-butoxycarbonyl)-2-formylmethylpiperazine

試薬・触媒・溶媒 2

HCID 178419074HCID 178419074、化合物触媒HCID 6344Dichloromethane溶媒

実験手順

In methylene chloride (150 ml) was dissolved 1,4-bis(tert-butoxycarbonyl)-2-(2-hydroxyethyl)piperazine. Under ice cooling, N-methylmorpholine (2.14 g) and tetra-n-propylammonium perruthenate (0.97 g) were added to the reaction mixture, followed by stirring at room temperature for 17 hours. The reaction mixture was then distilled off under reduced pressure. The residue was subjected to chromatography on a silica gel column (hexane:ethyl acetate=9:1 to 2:1), whereby the title compound (3.11 g) was obtained as colorless powder.

後処理

  1. distillationThe reaction mixture was then distilled off under reduced pressure
  2. customwas obtained as colorless powder

出典と根拠

ORDレコード
ord-e4e084b2d70246b787df9f9be46e0e48
出典データセット
uspto-grants-2004_06
特許番号
US06747023B1

反応ノート

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