1,4-Dioxane hydrochloride → HCID 86700081, compound

HRID 1428131Notes

Reaction equation

HRID 1428131 reaction equation
[NH2:1][C:2]1[C:7]([C:8]2[CH:13]=[CH:12][C:11]([NH:14][C:15]([C:17]3[C:22](=[O:23])[C:21]([C:24]4[CH:29]=[CH:28][C:27]([F:30])=[CH:26][CH:25]=4)=[CH:20][N:19]([CH2:31][C:32]([F:35])([F:34])[F:33])[CH:18]=3)=[O:16])=[CH:10][CH:9]=2)=[CH:6][C:5]([C:36]2[CH:41]=[CH:40][C:39]([O:42][CH3:43])=[C:38]([O:44][CH3:45])[CH:37]=2)=[CH:4][N:3]=1.[ClH:46].O1CCOCC1>C(O)C>[ClH:46].[NH2:1][C:2]1[C:7]([C:8]2[CH:9]=[CH:10][C:11]([NH:14][C:15]([C:17]3[C:22](=[O:23])[C:21]([C:24]4[CH:25]=[CH:26][C:27]([F:30])=[CH:28][CH:29]=4)=[CH:20][N:19]([CH2:31][C:32]([F:33])([F:34])[F:35])[CH:18]=3)=[O:16])=[CH:12][CH:13]=2)=[CH:6][C:5]([C:36]2[CH:41]=[CH:40][C:39]([O:42][CH3:43])=[C:38]([O:44][CH3:45])[CH:37]=2)=[CH:4][N:3]=1

Participants

4

Reactant 2

HCID 204431481,4-Dioxane hydrochlorideHCID 71698834HCID 71698834, compound

Product 1

HCID 86700081HCID 86700081, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

The compound of Step 3 of Example 9 (28.91 g) was suspended in ethanol (100 ml), and 4 N hydrochloric acid-dioxane (23.37 ml) was added at room temperature. After stirring at room temperature for two hours, the solvent was distilled off under reduced pressure, and the residue was recrystallized from ethanol/isopropyl ether (50 ml/150 ml). The resulting solid was collected by filtration, washed with isopropyl ether and then dried under reduced pressure to give 30.83 g of the title compound as a solid.

Workup

  1. distillationthe solvent was distilled off under reduced pressure
  2. customthe residue was recrystallized from ethanol/isopropyl ether (50 ml/150 ml)
  3. filtrationThe resulting solid was collected by filtration
  4. washwashed with isopropyl ether
  5. customdried under reduced pressure

Sources & evidence

ORD record
ord-8f638cdb49d04628b38f55cc0a62e3fc
Source dataset
uspto-grants-2015_01
Patent number
US08933103B2

Reaction notes

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