Hydrochloric Acid → HCID 66593992, compound

HRID 1093396Notes

Reaction equation

HRID 1093396 reaction equation
C(OC(=O)[NH:7][C:8]1([CH2:16][CH2:17][C:18]2[CH:23]=[CH:22][C:21]([O:24][CH2:25][CH2:26][CH2:27][C:28]3[S:29][C:30]([CH3:33])=[CH:31][CH:32]=3)=[C:20]([C:34]([F:37])([F:36])[F:35])[CH:19]=2)[CH2:13][O:12]C(C)(C)[O:10][CH2:9]1)(C)(C)C.[ClH:39]>C(O)C>[ClH:39].[NH2:7][C:8]([CH2:16][CH2:17][C:18]1[CH:23]=[CH:22][C:21]([O:24][CH2:25][CH2:26][CH2:27][C:28]2[S:29][C:30]([CH3:33])=[CH:31][CH:32]=2)=[C:20]([C:34]([F:37])([F:35])[F:36])[CH:19]=1)([CH2:13][OH:12])[CH2:9][OH:10]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 59407899HCID 59407899, compound

Product 1

HCID 66593992HCID 66593992, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Conditions

Temperature
80 °C

Procedure

Compound 48-4 (710 mg) was dissolved in ethanol (15 ml), concentrated hydrochloric acid (1.5 ml) was added, and the mixture was stirred at 80° C. for 2 hr. The reaction mixture was concentrated, and the residue was washed with diethyl ether to give a white powder. The white powder was purified by HPLC, the obtained residue was converted to hydrochloride by adding hydrogen chloride containing ether (1 mol/l, 15 ml), and the precipitate was collected by filtration and dried to give the object product (480 mg) as a white powder.

Workup

  1. concentrationThe reaction mixture was concentrated
  2. washthe residue was washed with diethyl ether
  3. customto give a white powder
  4. customThe white powder was purified by HPLC
  5. additionby adding hydrogen chloride
  6. additioncontaining ether (1 mol/l, 15 ml)
  7. filtrationthe precipitate was collected by filtration
  8. customdried

Sources & evidence

ORD record
ord-e1970241fcf8473e930741219d015939
Source dataset
uspto-grants-2012_03
Patent number
US08129361B2

Reaction notes

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