Phosphorus oxide (P4O10) → HCID 66807412, compound

HRID 1843878Notes

Reaction equation

HRID 1843878 reaction equation
C([O:3][C:4](=O)[NH:5][CH2:6][CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[C:14]([F:17])([F:16])[F:15])C.O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>O=P(Cl)(Cl)Cl>[F:15][C:14]([F:17])([F:16])[C:9]1[CH:10]=[CH:11][CH:12]=[C:13]2[C:8]=1[CH2:7][CH2:6][NH:5][C:4]2=[O:3]

Participants

4

Reactant 2

HCID 14812Phosphorus oxide (P4O10)HCID 66801879HCID 66801879, compound

Product 1

HCID 66807412HCID 66807412, compoundYield 9.1%

Reagents, catalysts & solvents 1

HCID 24813Phosphorus oxychlorideSolvent

Conditions

Temperature
115 °C

Procedure

Using the same procedure and workup as described in Example 1, step 4, [2-(2-trifluoromethyl-phenyl)-ethyl]-carbamic acid ethyl ester (I-22c: 1.2 g, 4.5977 mmol) in POCl3 (13 mL) was reacted with P2O5 (1.3 g, 9.195 mmol). The resulting mixture was stirred at 115° C. for 2 hours to afford the crude product. Purification by column chromatography on silica gel (60% ethylacetate in hexane) afforded 0.090 g of the product (9.1% yield).

Workup

  1. customto afford the crude product
  2. customPurification by column chromatography on silica gel (60% ethylacetate in hexane)

Sources & evidence

ORD record
ord-2d4a1337fd3944599dc34e807d420966
Source dataset
uspto-grants-2015_02
Patent number
US08946260B2

Reaction notes

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