Hydrochloric Acid → HCID 50938820, compound

HRID 269694Notes

Reaction equation

[ClH:1].Cl.C([N:7]([CH2:11][C@H:12]([OH:62])[CH2:13][C@@H:14]1[NH:32][C:31](=[O:33])[C@@H:30]([NH:34]C(OC(C)(C)C)=O)[CH2:29][C:28]2[CH:42]=[C:24]([CH:25]=[CH:26][C:27]=2[OH:43])[C:23]2=[CH:44][C:19](=[C:20]([OH:45])[CH:21]=[CH:22]2)[CH2:18][C@@H:17]([C:46]([NH:48][C@H:49]([C:55]([NH:57][CH2:58][CH2:59][NH2:60])=[O:56])[CH2:50][C@@H:51]([OH:54])[CH2:52][NH2:53])=[O:47])[NH:16][C:15]1=[O:61])C(=O)O)(C)(C)C.Cl>O1CCOCC1>[ClH:1].[ClH:1].[ClH:1].[ClH:1].[NH2:34][C@H:30]1[CH2:29][C:28]2[CH:42]=[C:24]([CH:25]=[CH:26][C:27]=2[OH:43])[C:23]2=[CH:44][C:19](=[C:20]([OH:45])[CH:21]=[CH:22]2)[CH2:18][C@@H:17]([C:46]([NH:48][C@H:49]([C:55]([NH:57][CH2:58][CH2:59][NH2:60])=[O:56])[CH2:50][C@@H:51]([OH:54])[CH2:52][NH2:53])=[O:47])[NH:16][C:15](=[O:61])[C@H:14]([CH2:13][C@@H:12]([OH:62])[CH2:11][NH2:7])[NH:32][C:31]1=[O:33]

Participants

Conditions

Temperature: 0 °C

Procedure

16 mg (0.02 mmol) of the compound from Example 172A are provided in 0.5 ml of dioxane and cooled to 0° C., and 1 ml of 4N hydrogen chloride in dioxane is added. The mixture is allowed to warm to room temperature and is stirred for 1 h. The mixture is then concentrated in vacuo and the residue is dried under high vacuum. Stirring with acetonitrile and collecting the precipitate which has separated out by filtration results in the title compound as a solid.

Workup

temperatureto warm to room temperature
concentrationThe mixture is then concentrated in vacuo
customthe residue is dried under high vacuum
stirringStirring with acetonitrile
customcollecting the precipitate which
customhas separated out by filtration

Sources & evidence

ORD record: ord-6684cc0a3c71465ea4ec87687bb550c8
Source dataset: uspto-grants-2008_11
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US07446102B2

Reaction notes

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