Lithium Hydroxide → HCID 67363378, compound

HRID 2064542Notes

Reaction equation

HRID 2064542 reaction equation
[C:1]([O:5][C:6]([N:8]([CH2:32][C:33]1[CH:42]=[CH:41][C:36]([C:37]([O:39]C)=[O:38])=[CH:35][CH:34]=1)[S:9]([C:12]1[CH:17]=[C:16]([C:18](=[O:30])[NH:19][N:20]2[C:28]3[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=3)[CH2:22][CH:21]2[CH3:29])[CH:15]=[CH:14][C:13]=1[Cl:31])(=[O:11])=[O:10])=[O:7])([CH3:4])([CH3:3])[CH3:2].[OH-].[Li+]>C(#N)C.O>[C:1]([O:5][C:6]([N:8]([CH2:32][C:33]1[CH:34]=[CH:35][C:36]([C:37]([OH:39])=[O:38])=[CH:41][CH:42]=1)[S:9]([C:12]1[CH:17]=[C:16]([C:18](=[O:30])[NH:19][N:20]2[C:28]3[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=3)[CH2:22][CH:21]2[CH3:29])[CH:15]=[CH:14][C:13]=1[Cl:31])(=[O:11])=[O:10])=[O:7])([CH3:2])([CH3:3])[CH3:4]

Participants

5

Reactant 2

HCID 3939Lithium HydroxideHCID 68431628HCID 68431628, compound

Product 1

HCID 67363378HCID 67363378, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolvent2×HCID 6342AcetonitrileSolvent

Procedure

Dissolve the compound obtained in Step A (1.30×10−3 mol) in a mixture of acetonitrile (45 ml) and water (9 ml). Add lithium hydroxide (1.30×10−2 mol) and heat at 50° C. with stirring. After heating for 5 hours, the dark-brown reaction mixture is poured into water (100 ml). Extract 3 times with ethyl acetate (50 ml). The organic phase is then washed with water and then with brine, dried over magnesium sulphate, filtered and evaporated to dryness under reduced pressure.

Workup

  1. temperatureAfter heating for 5 hours
  2. extractionExtract 3 times with ethyl acetate (50 ml)
  3. washThe organic phase is then washed with water
  4. dry with materialwith brine, dried over magnesium sulphate
  5. filtrationfiltered
  6. customevaporated to dryness under reduced pressure

Sources & evidence

ORD record
ord-57bc9be7f15a44b49ed2fd3e41eec9ad
Source dataset
uspto-grants-2012_10
Patent number
US08288433B2

Reaction notes

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