Phosphoric Acid → HCID 23649026, compound

HRID 1676902Notes

Reaction equation

HRID 1676902 reaction equation
[OH:1][P:2]([OH:5])([OH:4])=[O:3].O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.[NH2:20][C:21]1([CH2:40]O)[CH2:25][CH2:24][CH:23]([C:26]2[CH:31]=[CH:30][C:29]([CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH3:39])=[CH:28][CH:27]=2)[CH2:22]1>O>[P:2]([OH:5])([OH:4])([O:1][CH2:40][C:21]1([NH2:20])[CH2:25][CH2:24][CH:23]([C:26]2[CH:27]=[CH:28][C:29]([CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH3:39])=[CH:30][CH:31]=2)[CH2:22]1)=[O:3]

Participants

5

Reactant 3

HCID 1004Phosphoric AcidHCID 14812Phosphorus oxide (P4O10)2×HCID 11623636HCID 11623636, compound

Product 1

HCID 23649026HCID 23649026, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
100 °C

Procedure

1 mL of 85% H3PO4 was slowly added (by drops) into 0.5 g of P2O5, the acid-anhydride mixture was then heated at 100° C. for 1 hour under nitrogen protection. Another 0.5 g of P2O5 and 30 mg of alcohol 6 were added to the poly phosphoric acid and heated for 5 hours at 100° C. After cooling down to room temperature, 10 mL cold water (0° C.) was added to reaction mixture. The product precipitated out as white solid, was collected and washed with water. 31 mg (82%) of green colored product was collected after vacuum drying. MS only two peaks: M+1=384.4 with 304.4 (hydrolyzed back to 6).

Workup

  1. temperatureAfter cooling down to room temperature
  2. customThe product precipitated out as white solid
  3. customwas collected
  4. washwashed with water
  5. custom31 mg (82%) of green colored product was collected after vacuum
  6. customdrying

Sources & evidence

ORD record
ord-746b874dec4d4c0db55c03dca97a610f
Source dataset
uspto-grants-2011_08
Patent number
US08008286B2

Reaction notes

Loading…