Phosphorus oxide (P4O10) → HCID 66801876, compound

HRID 1843905Notes

Reaction equation

HRID 1843905 reaction equation
C([O:3][C:4](=O)[NH:5][CH2:6][CH2:7][C:8]1[CH:13]=[CH:12][C:11]([Cl:14])=[C:10]([F:15])[CH:9]=1)C.O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>O=P(Cl)(Cl)Cl>[Cl:14][C:11]1[C:10]([F:15])=[C:9]2[C:8]([CH2:7][CH2:6][NH:5][C:4]2=[O:3])=[CH:13][CH:12]=1

Participants

4

Reactant 2

HCID 14812Phosphorus oxide (P4O10)HCID 66803927HCID 66803927, compound

Product 1

HCID 66801876HCID 66801876, compoundYield 14.2%

Reagents, catalysts & solvents 1

HCID 24813Phosphorus oxychlorideSolvent

Procedure

Using the same reaction procedure and workup as described in example 1, [2-(4-chloro-3-fluoro-phenyl)-ethyl]-carbamic acid ethyl ester (I-33c: 1.3 g, 5.30 mmol) in POCl3 (10 mL) was reacted with P2O5 (1.5 g, 10.60 mmol) at 110° C. for 1 hour to afford the crude product. Purification by column chromatography on silica gel (30% ethylacetate in hexane) afforded 150 mg of the product (14% yield).

Workup

  1. customthe same reaction procedure
  2. customto afford the crude product
  3. customPurification by column chromatography on silica gel (30% ethylacetate in hexane)

Sources & evidence

ORD record
ord-96b00cfe185e44dfb7053e932bba0fe1
Source dataset
uspto-grants-2015_02
Patent number
US08946260B2

Reaction notes

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