Acetic Acid Mixture with Hydrobromic Acid → Hydrogen Bromide

HRID 1436032Notes

Reaction equation

HRID 1436032 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

  1. concentrationThe solvent is concentrated under reduced pressure
  2. 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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