Hydrochloric Acid → HCID 67040676, compound

HRID 605168Notes

Reaction equation

HRID 605168 reaction equation
C[O:2][C:3](=[O:33])[C:4]1[CH:9]=[CH:8][C:7]([S:10][C:11]2[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[CH:13][CH:12]=2)=[C:6]([NH:19][C:20]2[C:21]3[CH:29]=[CH:28][C:27]([CH:30]([CH3:32])[CH3:31])=[N:26][C:22]=3[N:23]=[CH:24][N:25]=2)[CH:5]=1.[OH-].[Na+].Cl>O1CCCC1>[CH:30]([C:27]1[CH:28]=[CH:29][C:21]2[C:20]([NH:19][C:6]3[CH:5]=[C:4]([CH:9]=[CH:8][C:7]=3[S:10][C:11]3[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[CH:13][CH:12]=3)[C:3]([OH:33])=[O:2])=[N:25][CH:24]=[N:23][C:22]=2[N:26]=1)([CH3:32])[CH3:31]

Participants

5

Conditions

Temperature
50 °C

Procedure

To the product from Example 136C (1.56 g, 3.4 mmol) in tetrahydrofuran (20 mL) was added 1N aqueous sodium hydroxide (10 mL, 10 mmol) and the reaction mixture heated at 50° C. for 3 hours. After cooling the reaction mixture to room temperature, the pH was adjusted to 6.5 with 1N aqueous hydrochloric acid and the resulting precipitate was removed by vacuum filtration. The product was dried under high vacuum overnight to provide the title compound as an off white solid (643 mg, 42%).

Workup

  1. temperatureAfter cooling the reaction mixture to room temperature
  2. customthe resulting precipitate was removed by vacuum filtration
  3. customThe product was dried under high vacuum overnight

Sources & evidence

ORD record
ord-dbb29918e7d544ee82855f0075395d17
Source dataset
uspto-grants-2011_03
Patent number
US07910595B2

Reaction notes

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