Hydrogen Bromide → HCID 68513745, compound

HRID 1971810Notes

Reaction equation

HRID 1971810 reaction equation
[CH:1]1([CH2:4][N:5]([CH2:28][CH:29]2[CH2:33][CH2:32][O:31][CH2:30]2)[C:6]2[C:7]([O:26][CH3:27])=[N:8][N:9]3[C:13]([C:14]4[C:21]([O:22][CH3:23])=[CH:20][C:17]([C:18]#[N:19])=[CH:16][C:15]=4[O:24][CH3:25])=[CH:12][S:11][C:10]=23)[CH2:3][CH2:2]1.[BrH:34]>CO>[BrH:34].[CH:1]1([CH2:4][N:5]([CH2:28][CH:29]2[CH2:33][CH2:32][O:31][CH2:30]2)[C:6]2[C:7]([O:26][CH3:27])=[N:8][N:9]3[C:13]([C:14]4[C:15]([O:24][CH3:25])=[CH:16][C:17]([C:18]#[N:19])=[CH:20][C:21]=4[O:22][CH3:23])=[CH:12][S:11][C:10]=23)[CH2:2][CH2:3]1

Participants

4

Procedure

To a mixture of 4-{7-[(cyclopropylmethyl)(tetrahydrofuran-3-ylmethyl)amino]-6-methoxypyrazolo[5,1-b][1,3]thiazol-3-yl}-3,5-dimethoxybenzonitrile (8.0 mg) and methanol (1 mL) was added hydrobromic acid (8.84M, 2.4 μL), and the mixture was stirred at room temperature for 1 hour and the solvent was distilled off under reduced pressure. Methanol (1 mL) was added to the residue and the solvent was distilled off under reduced pressure. Ethyl acetate (1 mL) was added to the resultant residue and the solvent was distilled off under reduced pressure and dried to obtain the titled compound (8.0 mg).

Workup

  1. distillationthe solvent was distilled off under reduced pressure
  2. additionMethanol (1 mL) was added to the residue
  3. distillationthe solvent was distilled off under reduced pressure
  4. additionEthyl acetate (1 mL) was added to the resultant residue
  5. distillationthe solvent was distilled off under reduced pressure
  6. customdried

Sources & evidence

ORD record
ord-7d46b6d5335e4aa2819b820ecf859d9a
Source dataset
uspto-grants-2013_04
Patent number
US08431603B2

Reaction notes

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