Lithium hydroxide, monohydrate → HCID 18689756, compound

HRID 1871967Notes

Reaction equation

HRID 1871967 reaction equation
[CH:1]1[C:11]2[CH:10]=[CH:9][C:8]3[CH:12]=[CH:13][CH:14]=[CH:15][C:7]=3[CH:6]([C:16]3[C:17](=[S:34])[NH:18][C:19](=[O:33])[N:20]([CH2:22][C:23]4[N:28]=[C:27]([C:29]([O:31]C)=[O:30])[CH:26]=[CH:25][CH:24]=4)[CH:21]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1.O.[OH-].[Li+]>CO.O>[CH:12]1[C:8]2[CH:9]=[CH:10][C:11]3[CH:1]=[CH:2][CH:3]=[CH:4][C:5]=3[CH:6]([C:16]3[C:17](=[S:34])[NH:18][C:19](=[O:33])[N:20]([CH2:22][C:23]4[N:28]=[C:27]([C:29]([OH:31])=[O:30])[CH:26]=[CH:25][CH:24]=4)[CH:21]=3)[C:7]=2[CH:15]=[CH:14][CH:13]=1

Participants

5

Reactant 2

HCID 168937Lithium hydroxide, monohydrateHCID 86755647HCID 86755647, compound

Product 1

HCID 18689756HCID 18689756, compound

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 962WaterSolvent

Procedure

A mixture of the product from step (vi) (1.37 g) and lithium hydroxide monohydrate (0.588 g) in methanol (20 ml) and water (15 ml) was stirred at room temperature for 3 hours. A precipitate formed which was filtered off and partitioned between ethyl acetate and 1N HCl. The organic phase was dried (MgSO4) and concentrated under reduced pressure to 10 ml. The product was precipitated by the addition of diethyl ether. Yield 0.56 g.

Workup

  1. customA precipitate formed which
  2. filtrationwas filtered off
  3. custompartitioned between ethyl acetate and 1N HCl
  4. dry with materialThe organic phase was dried (MgSO4)
  5. concentrationconcentrated under reduced pressure to 10 ml
  6. customThe product was precipitated by the addition of diethyl ether

Sources & evidence

ORD record
ord-5849f58d1b08495db9600ff31dd5cf9d
Source dataset
uspto-grants-2000_08
Patent number
US06107297

Reaction notes

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