1,4-Dioxane hydrochloride → Hydrochloric Acid

HRID 11875Notes

Reaction equation

HRID 11875 reaction equation
[C:1]1([CH2:11][NH:12][C:13](=[O:58])[C@@H:14]([NH:29][C:30]([C:32]2[C:41]3[C:36](=[CH:37][CH:38]=[CH:39][CH:40]=3)[C:35]([CH2:42][N:43](C(OC(C)(C)C)=O)[CH2:44][C:45]3[CH:50]=[CH:49][CH:48]=[CH:47][N:46]=3)=[CH:34][CH:33]=2)=[O:31])[CH2:15][CH2:16][CH2:17][NH:18][C@@H:19]2[C:28]3[N:27]=[CH:26][CH:25]=[CH:24][C:23]=3[CH2:22][CH2:21][CH2:20]2)[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1.[ClH:59].O1CCOCC1>CO>[ClH:59].[C:1]1([CH2:11][NH:12][C:13](=[O:58])[C@@H:14]([NH:29][C:30]([C:32]2[C:41]3[C:36](=[CH:37][CH:38]=[CH:39][CH:40]=3)[C:35]([CH2:42][NH:43][CH2:44][C:45]3[CH:50]=[CH:49][CH:48]=[CH:47][N:46]=3)=[CH:34][CH:33]=2)=[O:31])[CH2:15][CH2:16][CH2:17][NH:18][C@@H:19]2[C:28]3[N:27]=[CH:26][CH:25]=[CH:24][C:23]=3[CH2:22][CH2:21][CH2:20]2)[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1

Participants

5

Reactant 2

HCID 204431481,4-Dioxane hydrochlorideHCID 69638439HCID 69638439, compound

Product 2

HCID 313Hydrochloric AcidHCID 69638236HCID 69638236, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

The compound obtained in Example 90-2 (14.2 mg) was dissolved in methanol (0.3 ml), and 4 mol/l hydrochloric acid/dioxane solution (0.3 ml) was added to the solution. After the reaction for 3.5 hours, the reaction solution was concentrated. The residue obtained was purified by silica gel column chromatography (0.5 g, chloroform/methanol/water=7/3/0.5) and treated with hydrochloric acid to obtain hydrochloride of the title compound (8.1 mg) as a white solid.

Workup

  1. customAfter the reaction for 3.5 hours
  2. concentrationthe reaction solution was concentrated
  3. customThe residue obtained
  4. customwas purified by silica gel column chromatography (0.5 g, chloroform/methanol/water=7/3/0.5)
  5. additiontreated with hydrochloric acid

Sources & evidence

ORD record
ord-d904a5a2c0ac422f89170732fdcdba69
Source dataset
uspto-grants-2006_08
Patent number
US07098215B2

Reaction notes

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