Phosphorus oxychloride → HCID 89654102, compound

Reaction equation

[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

Participants

Reactant 2

HCID 24813Phosphorus oxychloride

HCID 89654098HCID 89654098, compound

Product 1

HCID 89654102HCID 89654102, compoundYield 100%

Conditions

Temperature: 90 °C

Procedure

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

Workup

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

Sources & evidence

ORD record: ord-dc887be935324e6fa66dc1fca179e980
Source dataset: uspto-grants-2014_07
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US08791114B2

Reaction notes

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