Lithium hydroxide, monohydrate → HCID 70296079, compound

HRID 1870960Notes

Reaction equation

HRID 1870960 reaction equation
C([O:5][C:6]([C:8]1[N:9](C(OC(C)(C)C)=O)[C:10]2[C:15]([C:16]=1[CH:17]([CH:19]1[C:23](=O)N(C(OC(C)(C)C)=O)[N:21]([CH:32]3C4CC5CC(C[CH:33]3C5)C4)[CH2:20]1)O)=[C:14]([Cl:42])[CH:13]=[C:12]([Cl:43])[CH:11]=2)=[O:7])(C)(C)C.[OH2:51].[OH-].[Li+]>C(O)C>[Cl:42][C:14]1[CH:13]=[C:12]([Cl:43])[CH:11]=[C:10]2[C:15]=1[C:16](/[CH:17]=[C:19]1/[C:20](=[O:51])[NH:21][CH2:32][CH2:33][CH2:23]/1)=[C:8]([C:6]([OH:5])=[O:7])[NH:9]2

Participants

4

Reactant 2

HCID 168937Lithium hydroxide, monohydrateHCID 18694373HCID 18694373, compound

Product 1

HCID 70296079HCID 70296079, compoundYield 176.8%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

Example 4 (490 mg) and lithium hydroxide monohydrate (200 mg) were dissolved in ethanol (95%) (20 ml) and the resulting solution refluxed for 1.5 h. The solvent was evaporated and the residue treated at 50° with 6 M hydrochloric acid for 30 min, then at room temperature for further 30 min. The resulting white solid was filtered, washed and vacuum dried to yield the title compound (400 mg) as a white solid.

Workup

  1. temperaturethe resulting solution refluxed for 1.5 h
  2. customThe solvent was evaporated
  3. additionthe residue treated at 50° with 6 M hydrochloric acid for 30 min
  4. filtrationThe resulting white solid was filtered
  5. washwashed
  6. customvacuum dried

Sources & evidence

ORD record
ord-b56b3599240f491ab83cb6d766d0b7fc
Source dataset
uspto-grants-2000_08
Patent number
US06100289

Reaction notes

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