Hydrochloric Acid → HCID 69893385, compound

HRID 353201Notes

Reaction equation

HRID 353201 reaction equation
[CH3:1][O:2][CH2:3][CH2:4][N:5]([CH2:23][C:24]1[CH:40]=[CH:39][C:27]([O:28][C:29]([CH3:38])([CH3:37])[C:30]([O:32]C(C)(C)C)=[O:31])=[CH:26][CH:25]=1)[CH2:6][C:7]([NH:9][C:10]1[CH:15]=[CH:14][C:13]([CH:16]([CH3:18])[CH3:17])=[CH:12][C:11]=1[C:19]([F:22])([F:21])[F:20])=[O:8].[ClH:41].C(OCC)C>C(OCC)(=O)C>[ClH:41].[CH3:1][O:2][CH2:3][CH2:4][N:5]([CH2:23][C:24]1[CH:25]=[CH:26][C:27]([O:28][C:29]([CH3:38])([CH3:37])[C:30]([OH:32])=[O:31])=[CH:39][CH:40]=1)[CH2:6][C:7]([NH:9][C:10]1[CH:15]=[CH:14][C:13]([CH:16]([CH3:18])[CH3:17])=[CH:12][C:11]=1[C:19]([F:22])([F:21])[F:20])=[O:8]

Participants

5

Procedure

0.4 g (0.78 mmol) of the compound from Example 3-7 are dissolved in 4 ml of ethyl acetate. At 40° C., first 8 ml of 1N hydrochloric acid (in diethyl ether) and then 12 ml of diethyl ether are added. The mixture is allowed to stand at 4° C. for one hour. The precipitated crystals are filtered off with suction, washed with a mixture of ethyl acetate and diethyl ether (ratio 1:1) and then dried at 40° C. under reduced pressure for 20 hours. This gives 0.362 g (84.5% of theory) of the title compound.

Workup

  1. filtrationThe precipitated crystals are filtered off with suction
  2. washwashed with a mixture of ethyl acetate and diethyl ether (ratio 1:1)
  3. customdried at 40° C. under reduced pressure for 20 hours

Sources & evidence

ORD record
ord-bcd6caa364784d78b39853b52fe1fa29
Source dataset
uspto-grants-2004_06
Patent number
US06750236B2

Reaction notes

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