Acetic Acid Mixture with Hydrobromic Acid → Hydrogen Bromide
Reaction equation
[BrH:1].C(O)(=O)C.C(OC([NH:13][CH:14]1[CH2:18][CH2:17][N:16]([S:19]([C:22]2[C:23]3[C:24]([O:32]C)=[CH:25][N:26]=[CH:27][C:28]=3[CH:29]=[CH:30][CH:31]=2)(=[O:21])=[O:20])[CH2:15]1)=O)(C)(C)C>>[NH2:13][CH:14]1[CH2:18][CH2:17][N:16]([S:19]([C:22]2[C:23]3[C:24]([OH:32])=[CH:25][N:26]=[CH:27][C:28]=3[CH:29]=[CH:30][CH:31]=2)(=[O:20])=[O:21])[CH2:15]1.[BrH:1]Participants
4
Procedure
30% Hydrogen bromide/acetic acid (1.5 ml, Tokyo Kasei Kogyo) is gradually added with Intermediate 13 (45 mg) obtained in Example 15, Step A at 0° C., and the mixture is stirred at the same temperature for 30 minutes. The solvent is concentrated under reduced pressure, and the obtained solid is collected by filtration to obtain the title compound as hydrobromide (13 mg (predictive yield)).
Workup
- concentrationThe solvent is concentrated under reduced pressure
- filtrationthe obtained solid is collected by filtration
Sources & evidence
- ORD record
- ord-234b9961e29948ce8d54acff8cb09d5d
- Source dataset
- uspto-grants-2009_11
- Patent number
- US07618984B2
Reaction notes
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