Phosphorus oxychloride → HCID 89654102、化合物

反応式

[ClH:1].[CH3:2][C:3]1([CH3:9])[NH:7][NH:6][C:5](=O)[CH2:4]1.O=P(Cl)(Cl)[Cl:12]>>[ClH:12].[Cl:1][C:5]1[CH2:4][C:3]([CH3:9])([CH3:2])[NH:7][N:6]=1

参加物

反応物 2

HCID 24813Phosphorus oxychloride

HCID 89654098HCID 89654098、化合物

生成物 1

HCID 89654102HCID 89654102、化合物収率 100%

反応条件

温度: 90 °C

実験手順

A round 50 mL round bottom flask equipped with stir bar, Vigreux column and nitrogen inlet was charged with 5,5-dimethyl-pyrazolidin-3-one.Hydrochloride (300 mg, 2.0 mmol) and POCl3 (4 mL). The mixture was heated at 90° C. for 3 h. LC-MS showed consumption of SM. The POCl3 was evaporated under reduced pressure and trace POCl3 was removed under high vacuum for 30 min. Amount obtained: 336 mg, 2.0 mmol, 100% yield. The material was used as in the next step. Step 4

後処理

customA round 50 mL round bottom flask equipped
customconsumption of SM
customThe POCl3 was evaporated under reduced pressure and trace POCl3
customwas removed under high vacuum for 30 min
customAmount obtained

出典と根拠

ORDレコード: ord-dc887be935324e6fa66dc1fca179e980
出典データセット: uspto-grants-2014_07
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US08791114B2

反応ノート

読み込み中…

参加物