Hydrochloric Acid → HCID 136171790, compound

HRID 1700108Notes

Reaction equation

HRID 1700108 reaction equation
Cl.[CH3:2][O:3][N:4]=[C:5]([C:7]1[C:8](=[O:29])[O:9][C:10]2[C:20]([CH3:21])=[C:19]([O:22]C3CCCCO3)[CH:18]=[CH:17][C:11]=2[C:12]=1[O:13][CH2:14][CH:15]=[CH2:16])[CH3:6].O1CCCC1>CCCCCC.C(OCC)(=O)C>[OH:22][C:19]1[CH:18]=[CH:17][C:11]2[C:12]([O:13][CH2:14][CH:15]=[CH2:16])=[C:7]([C:5](=[N:4][O:3][CH3:2])[CH3:6])[C:8](=[O:29])[O:9][C:10]=2[C:20]=1[CH3:21]

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 131723121HCID 131723121, compound

Product 1

HCID 136171790HCID 136171790, compound

Reagents, catalysts & solvents 1

HCID 21226206Ethyl acetate hexaneSolvent

Procedure

10 ml of a 1M aqueous solution of hydrochloric acid is added to a solution containing 1 g of the product prepared in Stage C and 20 ml of tetrahydrofuran. Agitation is carried out for 7 hours at ambient temperature followed by dilution with 50 ml of a hexane-ethyl acetate mixture (1-1). The phases are separated and the aqueous phase is extracted with a hexane-ethyl acetate mixture (1-1). The organic phases are combined and washed with a 1M solution of sodium dihydrogen phosphate, followed by drying, filtering and concentrating to dryness. The residue is triturated with a hexane-ethyl acetate mixture (4-1). After separating and drying 770 mg of product is collected.

Workup

  1. customThe phases are separated
  2. extractionthe aqueous phase is extracted with a hexane-ethyl acetate mixture (1-1)
  3. washwashed with a 1M solution of sodium dihydrogen phosphate
  4. customby drying
  5. filtrationfiltering
  6. concentrationconcentrating to dryness
  7. customThe residue is triturated with a hexane-ethyl acetate mixture (4-1)
  8. customAfter separating
  9. dry with materialdrying 770 mg of product
  10. customis collected

Sources & evidence

ORD record
ord-bbc199fedbeb4ffbb651b40b8eac7560
Source dataset
uspto-grants-2002_02
Patent number
US06350733B1

Reaction notes

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