Hydrogen Bromide → HCID 69735974, compound

HRID 497387Notes

Reaction equation

HRID 497387 reaction equation
C[O:2][C:3]([C:5]1[C:16]2[C:15]3[N:11]([CH:12]=[CH:13][N:14]=3)[CH2:10][CH2:9][C:8]=2[NH:7][CH:6]=1)=[O:4].[BrH:17]>>[BrH:17].[N:14]1[CH:13]=[CH:12][N:11]2[C:15]=1[C:16]1[C:5]([C:3]([OH:4])=[O:2])=[CH:6][NH:7][C:8]=1[CH2:9][CH2:10]2

Participants

3

Reactant 2

HCID 260Hydrogen BromideHCID 20605631HCID 20605631, compound

Product 1

HCID 69735974HCID 69735974, compound

Procedure

A solution of 5,6-dihydro-4H-1,3a,6-triaza-as-indacene-8-carboxylic acid methyl ester (516 mg) and 48% hydrobromic acid (5 mL) is heated at 60° for 60 hours. The mixture is cooled to room temperature and concentrated in vacuo. The residue is slurried with diethyl ether and the ether is decanted off. This is repeated until no more color is visible in the ether layer. The remaining solid is dried in vacuo to give 5,6-dihydro-4H-1,3a,6-triaza-as-indacene-8-carboxylic acid hydrobromide, 350 mg, brown solid: 1H NMR(DMSO-d6) 3.17 (2H, t), 4.40 (2H, t), 7.35 (1H, d), 7.57 (1H, d), 7.63 (1H, s), 12.34 (1H, s), 12.45 (1H, s).

Workup

  1. concentrationconcentrated in vacuo
  2. customthe ether is decanted off
  3. customThe remaining solid is dried in vacuo

Sources & evidence

ORD record
ord-6f7025ef8b134be0b03286e5ce9b585e
Source dataset
uspto-grants-2005_09
Patent number
US06949562B2

Reaction notes

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