Hydrochloric Acid → HCID 67954047, compound

HRID 1916848Notes

Reaction equation

HRID 1916848 reaction equation
[CH:1]([C:4]1[N:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]2=[N:6][C:5]=1[C:13]([O-:15])=[O:14])([CH3:3])[CH3:2].[Li+].[ClH:17].[Cl-].[Li+]>O>[ClH:17].[CH:1]([C:4]1[N:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]2=[N:6][C:5]=1[C:13]([OH:15])=[O:14])([CH3:3])[CH3:2]

Participants

5

Procedure

A solution of compound 4-C (0.764 g, 3.64 mmol) in water (7 mL) was treated with 1N HCl (7.45 mL, 7.45 mmol), and the resultant solution was filtered then frozen on a dry ice/acetone bath. The water was lyophilized away to leave a mixture of compound 4-D with lithium chloride (1.01 g, 98%) as a colorless solid, used as is in the subsequent reaction. 1H-NMR (CD3OD): δ 8.84 (d, J=7.1 Hz, 1H), 7.74-7.89 (m, 2H), 7.35-7.40 (m, 1H), 4.32-4.43 (m, 1H), 1.55 (d, J=7.3 Hz, 6H); MS: m/z 205.2 (MH+).

Workup

  1. filtrationthe resultant solution was filtered
  2. temperaturethen frozen on a dry ice/acetone bath
  3. customto leave
  4. customused as is in the subsequent reaction

Sources & evidence

ORD record
ord-6af0ce7443ce46c78e18b06a301ffee1
Source dataset
uspto-grants-2013_12
Patent number
US08618150B2

Reaction notes

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