Lithium Hydroxide → HCID 86699626, compound

HRID 68317Notes

Reaction equation

HRID 68317 reaction equation
[F:1][C:2]([F:29])([F:28])[C:3]1[CH:27]=[CH:26][C:6]([CH2:7][O:8][N:9]=[C:10]([C:13]2[CH:18]=[CH:17][C:16]([NH:19][CH2:20][C:21]([O:23]CC)=[O:22])=[CH:15][CH:14]=2)[CH2:11][CH3:12])=[CH:5][CH:4]=1.[OH-].[Li+]>C1COCC1.O>[F:1][C:2]([F:28])([F:29])[C:3]1[CH:27]=[CH:26][C:6]([CH2:7][O:8][N:9]=[C:10]([C:13]2[CH:18]=[CH:17][C:16]([NH:19][CH2:20][C:21]([OH:23])=[O:22])=[CH:15][CH:14]=2)[CH2:11][CH3:12])=[CH:5][CH:4]=1

Participants

5

Conditions

Temperature
25 °C

Procedure

To a solution of the product of step 3 (2.2 g, 5.39 mmoles) in THF (10 ml), a solution of lithium hydroxide (0.45 g, 10.77 mmoles) in water (10 mL) was added and the reaction mixture was stirred at 25° C. for 3 hours. The solvents were evaporated under reduced pressure. The residue was dissolved in water and neutralized to pH 6 with 1N HCl. Solid seperated was filtered, washed with water and dried over CaCl2 under vacuum to give 1.64 g (82%) of title product.

Workup

  1. customThe solvents were evaporated under reduced pressure
  2. dissolutionThe residue was dissolved in water and neutralized to pH 6 with 1N HCl
  3. customSolid seperated
  4. filtrationwas filtered
  5. washwashed with water
  6. dry with materialdried over CaCl2 under vacuum

Sources & evidence

ORD record
ord-d067f3eb729143d0be392031cd37277b
Source dataset
uspto-grants-2014_09
Patent number
US08822414B2

Reaction notes

Loading…