Phosphorus oxide (P4O10) → HCID 66807377, compound

HRID 1843909Notes

Reaction equation

HRID 1843909 reaction equation
C([O:3][C:4](=O)[NH:5][CH2:6][CH2:7][C:8]1[CH:13]=[CH:12][C:11]([F:14])=[C:10]([Cl:15])[CH:9]=1)C.O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>O=P(Cl)(Cl)Cl>[Cl:15][C:10]1[C:11]([F:14])=[CH:12][CH:13]=[C:8]2[C:9]=1[C:4](=[O:3])[NH:5][CH2:6][CH2:7]2

Participants

4

Reactant 2

HCID 14812Phosphorus oxide (P4O10)HCID 66801676HCID 66801676, compound

Product 1

HCID 66807377HCID 66807377, compoundYield 21.98%

Reagents, catalysts & solvents 1

HCID 24813Phosphorus oxychlorideSolvent

Procedure

Using the same reaction procedure and workup as described in Example 1, [2-(3-chloro-4-fluoro-phenyl)-ethyl]-carbamic acid ethyl ester (I-34c: 1.4 g, 5.7142 mmol) in POCl3 (11.4 mL) was reacted with P2O5 (1.62 g, 11.4285 mmol) at 110° C. for 2 hours to afford the crude product. Purification by column chromatography on silica gel (35% ethylacetate in hexane) afforded 250 mg of the product (21.98% yield).

Workup

  1. customthe same reaction procedure
  2. customto afford the crude product
  3. customPurification by column chromatography on silica gel (35% ethylacetate in hexane)

Sources & evidence

ORD record
ord-45b3bd9aa9124ee3a546a537259a30ab
Source dataset
uspto-grants-2015_02
Patent number
US08946260B2

Reaction notes

Loading…