Phosphoric Acid → HCID 23649026, compound

HRID 2354543Notes

Reaction equation

HRID 2354543 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

Conditions

Temperature
100 °C

Procedure

1 mL 85% H3PO4 was slowly drop added 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 6 were added to the poly phosphoric acid and heated for 5 hours at 100° C. After cooling down to RT, 10 mL icy cold water was added to reaction mixture. Product precipitated out as white solid. The product was collected and washed with water. 31 mg (82%) green colored product was collected after vacuum dry. MS only two peaks: M+1=384.4 with 304.4 (hydrolyzed back to 6).

Workup

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

Sources & evidence

ORD record
ord-50b5fcedf26e40528de6d2aa5e6dad32
Source dataset
uspto-grants-2010_07
Patent number
US07754703B2

Reaction notes

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