Phosphorus oxide (P4O10) → HCID 86595412, compound

HRID 1593420Notes

Reaction equation

HRID 1593420 reaction equation
[CH3:1][N:2]([CH3:36])[CH2:3][CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([C:12](=[O:35])[CH2:13][CH:14]([C:29]2[CH:34]=[CH:33][N:32]=[CH:31][CH:30]=2)[C:15]([C:17]2[CH:18]=[C:19]3[C:23](=[CH:24][CH:25]=2)[C:22](=[N:26][O:27][CH3:28])[CH2:21][CH2:20]3)=O)=[CH:8][CH:7]=1.O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.C(=O)([O-])O.[Na+]>CS(O)(=O)=O>[CH3:28][O:27][N:26]=[C:22]1[C:23]2[C:19](=[CH:18][C:17]([C:15]3[O:35][C:12]([C:9]4[CH:8]=[CH:7][C:6]([O:5][CH2:4][CH2:3][N:2]([CH3:36])[CH3:1])=[CH:11][CH:10]=4)=[CH:13][C:14]=3[C:29]3[CH:30]=[CH:31][N:32]=[CH:33][CH:34]=3)=[CH:25][CH:24]=2)[CH2:20][CH2:21]1

Participants

5

Reactant 3

HCID 14812Phosphorus oxide (P4O10)HCID 516892Sodium BicarbonateHCID 86595407HCID 86595407, compound

Product 1

HCID 86595412HCID 86595412, compoundYield 96.6%

Reagents, catalysts & solvents 1

HCID 6395Methanesulfonic AcidSolvent

Procedure

The product of Example 1 Step 4 (0.30 mg, 0.62 mmol) was added to a stirred suspension of phosphorus pentoxide (1 g) in dry methane sulphonic acid (5 ml). After stirring at room temperature for 2 hours the reaction mixture was cautiously poured into a stirred solution of saturated aqueous sodium hydrogen carbonate. The mixture was extracted with ethyl acetate and the organic phase washed with water and saturated brine, dried (MgSO4) and concentrated in vacuo to afford the title compound (0.28 g, 96%); MS(ES+) m/e 468 [M+H]+.

Workup

  1. extractionThe mixture was extracted with ethyl acetate
  2. washthe organic phase washed with water and saturated brine
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated in vacuo

Sources & evidence

ORD record
ord-bed2e5b6e4584709a6c7ac8a0e76363d
Source dataset
uspto-grants-2007_11
Patent number
US07297694B2

Reaction notes

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