Hydrochloric Acid → HCID 67417544, compound

HRID 2406040Notes

Reaction equation

HRID 2406040 reaction equation
C(OC(=O)[NH:7][C:8]([CH2:31][OH:32])([CH2:29][OH:30])[CH2:9][CH2:10][C:11]1[CH:16]=[CH:15][C:14]([S:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24])=[C:13]([C:25]([F:28])([F:27])[F:26])[CH:12]=1)(C)(C)C.O1CCOCC1.[ClH:40]>C(Cl)Cl>[ClH:40].[NH2:7][C:8]([CH2:9][CH2:10][C:11]1[CH:16]=[CH:15][C:14]([S:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24])=[C:13]([C:25]([F:28])([F:26])[F:27])[CH:12]=1)([CH2:29][OH:30])[CH2:31][OH:32]

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 57704543HCID 57704543, compound

Product 1

HCID 67417544HCID 67417544, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

Compound 24-1 (390 mg) was dissolved in methylene chloride (5 ml), dioxane containing hydrogen chloride (4 mol/l, 5 ml) was added, and the mixture was stirred at room temperature for 4 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 preparative HPLC, ether containing hydrogen chloride (1 mol/l, 15 ml) was added to the obtained residue to give a hydrochloride. The precipitate was collected by filtration and dried to give the object product (200 mg) as a white powder.

Workup

  1. additionwas added
  2. concentrationThe reaction mixture was concentrated
  3. washthe residue was washed with diethyl ether
  4. customto give a white powder
  5. customThe white powder was purified by preparative HPLC, ether
  6. additioncontaining hydrogen chloride (1 mol/l, 15 ml)
  7. additionwas added to the obtained residue

Sources & evidence

ORD record
ord-a68a937842314eb0aad600a0adf7fee4
Source dataset
uspto-grants-2014_08
Patent number
US08809304B2

Reaction notes

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