Oxalyl chloride → Quinuclidin-4-ylcarbonyl chloride hydrochloride

HRID 1923397ノート

反応式

HRID 1923397 の反応式
[ClH:1].[N:2]12[CH2:9][CH2:8][C:5]([C:10](O)=[O:11])([CH2:6][CH2:7]1)[CH2:4][CH2:3]2.C(Cl)(=O)C([Cl:16])=O>ClCCl.CN(C)C=O>[ClH:16].[N:2]12[CH2:9][CH2:8][C:5]([C:10]([Cl:1])=[O:11])([CH2:6][CH2:7]1)[CH2:4][CH2:3]2

参加物

5

反応物 2

HCID 65578Oxalyl chlorideHCID 667378251-Azabicyclo(2.2.2)octane-4-carboxylic acid hydrochloride

生成物 1

HCID 13760941Quinuclidin-4-ylcarbonyl chloride hydrochloride

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide触媒HCID 6344Dichloromethane溶媒2 回

実験手順

Quinuclidine-4-carboxylic acid hydrochloride (0.192 g, 0.001 mole) was suspended in dichloromethane (5 ml) and dimethylformamide (1 drop) and oxalyl chloride (0.436 ml. 0.635 g, 0.005 mole) were added. The resulting suspension was heated to reflux under an atmosphere of argon for six hours. Following concentration of the suspension in vacuo the residue was suspended in dichloromethane, concentrated in vacuo and finally dried in vacuo to give the title compound as a pale brown solid.

後処理

  1. temperatureThe resulting suspension was heated
  2. temperatureto reflux under an atmosphere of argon for six hours
  3. concentrationconcentrated in vacuo
  4. customfinally dried in vacuo

出典と根拠

ORDレコード
ord-f8c36db196cd4f3cbec6c561bc16468e
出典データセット
uspto-grants-2012_05
特許番号
USRE043390E1

反応ノート

読み込み中…