1,4-Dioxane hydrochloride → HCID 86700081, compound

HRID 1428129Notes

Reaction equation

HRID 1428129 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 (15.7 g) was suspended in ethanol (50 ml), and 4 N hydrochloric acid-dioxane (12.69 ml) was added at room temperature. After stirring at room temperature, the solvent was distilled off under reduced pressure. The residue was suspended in acetonitrile, and the suspension was stirred overnight. The resulting solid was collected by filtration, and the solid was then suspended in hexane, followed by stirring for three days. The resulting solid was collected by filtration and then dried under reduced pressure to give 15.7 g of the title compound as a solid.

Workup

  1. distillationthe solvent was distilled off under reduced pressure
  2. stirringthe suspension was stirred overnight
  3. filtrationThe resulting solid was collected by filtration
  4. stirringby stirring for three days
  5. filtrationThe resulting solid was collected by filtration
  6. customdried under reduced pressure

Sources & evidence

ORD record
ord-bf22a91c626143d6bd6dafd0d4fa3461
Source dataset
uspto-grants-2015_01
Patent number
US08933103B2

Reaction notes

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