Lithium Hydroxide → HCID 86685839, compound

HRID 1045806Notes

Reaction equation

HRID 1045806 reaction equation
[Cl:1][C:2]1[N:7]=[C:6]([N:8]2[CH2:12][C@@H:11]([C:13]3[CH:18]=[CH:17][C:16]([F:19])=[CH:15][C:14]=3[F:20])[C@H:10]([C:21]([O:23]C)=[O:22])[CH2:9]2)[CH:5]=[CH:4][CH:3]=1.[Li+].[OH-].OS([O-])(=O)=O.[Na+]>C1COCC1>[Cl:1][C:2]1[N:7]=[C:6]([N:8]2[CH2:12][C@@H:11]([C:13]3[CH:18]=[CH:17][C:16]([F:19])=[CH:15][C:14]=3[F:20])[C@H:10]([C:21]([OH:23])=[O:22])[CH2:9]2)[CH:5]=[CH:4][CH:3]=1

Participants

5

Reactant 3

HCID 3939Lithium HydroxideHCID 516919Sodium BisulfateHCID 86685837HCID 86685837, compound

Product 1

HCID 86685839HCID 86685839, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

The product from step A (41 mg, 0.116 mmol) in THF (2.0 ml) was treated with 1M aqueous LiOH (0.349 ml, 0.349 mmol) at rt. The mixture was stirred at rt for 12 h, poured into 2M aq NaHSO4 and extracted with MTBE. The combined organics were dried with anhydrous Na2SO4, filtered and concentrated to afford the title compound which was used without further purification. HPLC/MS: 339.1/340.9 (M+1); Rt=1.16 min (LC2).

Workup

  1. extractionextracted with MTBE
  2. dry with materialThe combined organics were dried with anhydrous Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated

Sources & evidence

ORD record
ord-3f280428bf4b4d4b91936936f3cf1a34
Source dataset
uspto-grants-2013_10
Patent number
US08569299B2

Reaction notes

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