Phosphorus oxychloride → HCID 89654102, 화합물

반응식

[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

참가 물질

반응물 2

HCID 24813Phosphorus oxychloride

HCID 89654098HCID 89654098, 화합물

생성물 1

HCID 89654102HCID 89654102, 화합물수율 100%

반응 조건

온도: 90 °C

실험 절차

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

후처리

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

출처 및 근거

ORD 기록: ord-dc887be935324e6fa66dc1fca179e980
출처 데이터셋: uspto-grants-2014_07
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US08791114B2

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