Hydrochloric Acid → HCID 131713413, compound

HRID 1903247Notes

Reaction equation

HRID 1903247 reaction equation
[F:1][CH:2]([F:25])[CH:3]([NH:17][CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[CH2:4][CH2:5][N:6]1C(=O)C2=CC=CC=C2C1=O.[ClH:26]>>[ClH:26].[ClH:26].[F:1][CH:2]([F:25])[CH:3]([NH:17][CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[CH2:4][CH2:5][NH2:6]

Participants

3

Reactant 2

HCID 313Hydrochloric AcidHCID 20468458HCID 20468458, compound

Product 1

HCID 131713413HCID 131713413, compound

Conditions

Temperature
110 °C

Procedure

A solution of N-(4,4-difluoro-3-benzylaminobutyl) phthalimide (0.585 g, 1.72 mM) prepared as in Step D in concentrated hydrochloric acid (50 ml) is heated at 110° C. for 15 hours. The solvent is evaporated in vacuo, and the residue is taken up in cold water (50 ml). The aqueous phase is filtered and concentrated in vacuo, washed three times with diethyl ether, and then evaporated to dryness. The oily residue is triturated several times with isopropanol. The solvent is removed in vacuo yielding a white foam: 0.490 g (quantitative yield) of the required compound.

Workup

  1. customThe solvent is evaporated in vacuo
  2. filtrationThe aqueous phase is filtered
  3. concentrationconcentrated in vacuo
  4. washwashed three times with diethyl ether
  5. customevaporated to dryness
  6. customThe oily residue is triturated several times with isopropanol
  7. customThe solvent is removed in vacuo
  8. customyielding a white foam

Sources & evidence

ORD record
ord-6647d4f12489491da1da267dc1bdf51e
Source dataset
uspto-grants-1984_03
Patent number
US04435425

Reaction notes

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