Lithium Hydroxide → HCID 67364661, compound

HRID 2064544Notes

Reaction equation

HRID 2064544 reaction equation
[C:1]([O:5][C:6]([N:8]([CH2:32][C:33]1[CH:42]=[CH:41][CH:40]=[CH:39][C:34]=1[C:35]([O:37]C)=[O:36])[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:42]=[CH:41][CH:40]=[CH:39][C:34]=1[C:35]([OH:37])=[O:36])[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 68430502HCID 68430502, compound

Product 1

HCID 67364661HCID 67364661, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolvent2×HCID 6342AcetonitrileSolvent

Procedure

Dissolve the compound obtained in Step A (1.26×10−3 mol) in a mixture of acetonitrile (45 ml) and water (9 ml). Add lithium hydroxide (1.26×10−2 mol) and heat at 50° C. with stirring. After heating for 5 hours and 30 minutes, 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 and 30 minutes
  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-effbb711914c44f3adb37f02b3c10c23
Source dataset
uspto-grants-2012_10
Patent number
US08288433B2

Reaction notes

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