Hydrochloric Acid → HCID 69513669, compound

HRID 1593488Notes

Reaction equation

HRID 1593488 reaction equation
FC(F)(F)C(O)=[O:4].CON=[C:11]1[C:19]2[C:14](=[CH:15][C:16]([C:20]3[CH:21]=[C:22]([C:31]([OH:33])=[O:32])[O:23][C:24]=3[C:25]3[CH:30]=[CH:29][N:28]=[CH:27][CH:26]=3)=[CH:17][CH:18]=2)[CH2:13][CH2:12]1.O1CCOCC1.[ClH:40]>CC(C)=O>[ClH:40].[O:4]=[C:11]1[C:19]2[C:14](=[CH:15][C:16]([C:20]3[CH:21]=[C:22]([C:31]([OH:33])=[O:32])[O:23][C:24]=3[C:25]3[CH:26]=[CH:27][N:28]=[CH:29][CH:30]=3)=[CH:17][CH:18]=2)[CH2:13][CH2:12]1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 86760576HCID 86760576, compound

Product 1

HCID 69513669HCID 69513669, compound

Reagents, catalysts & solvents 1

HCID 180AcetoneSolvent2×

Procedure

The product from Step 3 (5.46 g, 11.7 mmol) was suspended in 5M hydrochloric acid (50 ml), dioxane (50 ml) and acetone (10 ml). The suspension was heated to reflux for 30 minutes, whereupon the suspended solids dissolved. The heating was continued for a further 90 minutes before the mixture was cooled, diluted with acetone (100 ml) and evaporated in vacuo to a wet solid. The solid was dried by repeatedly (×3) suspending in toluene and evaporating to dryness.

Workup

  1. temperatureThe suspension was heated
  2. temperatureto reflux for 30 minutes, whereupon the suspended solids
  3. dissolutiondissolved
  4. temperaturewas cooled
  5. customevaporated in vacuo to a wet solid
  6. customThe solid was dried by repeatedly (×3)
  7. customevaporating to dryness

Sources & evidence

ORD record
ord-2efc050c4bd747428df3ac9169db64ac
Source dataset
uspto-grants-2007_11
Patent number
US07297693B2

Reaction notes

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