HCID 54331584, compound → HCID 53967250, compound

HRID 1870824Notes

Reaction equation

HRID 1870824 reaction equation
[CH3:1][C:2]([C:21]1[CH:25]=[C:24]([N:26]=[C:27]([NH2:34])[N:28]2[CH2:33][CH2:32][O:31][CH2:30][CH2:29]2)[O:23][N:22]=1)([C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([C:10]2([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)OCC[O:11]2)[CH:5]=1)[CH3:3]>C(O)(=O)C>[NH2:34][C:27]([N:28]1[CH2:33][CH2:32][O:31][CH2:30][CH2:29]1)=[N:26][C:24]1[O:23][N:22]=[C:21]([C:2]([C:4]2[CH:5]=[C:6]([C:10]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)=[O:11])[CH:7]=[CH:8][CH:9]=2)([CH3:3])[CH3:1])[CH:25]=1

Participants

3

Reactant 1

HCID 54331584HCID 54331584, compound

Product 1

HCID 53967250HCID 53967250, compoundYield 104.2%

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

The compound (8.8 mg) obtained in Example 131 was dissolved in 90% aqueous acetic acid solution (2 ml), followed by stirring for 40 hours. The reaction solution was extracted with ethyl acetate, and the extract solution was washed with a saturated aqueous sodium chloride solution, dried over sodium sulfate and thereafter concentrated under reduced pressure. The resulting residue was purified by a silica gel column chromatography to obtain the desired compound (8.3 mg).

Workup

  1. extractionThe reaction solution was extracted with ethyl acetate
  2. washthe extract solution was washed with a saturated aqueous sodium chloride solution
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe resulting residue was purified by a silica gel column chromatography

Sources & evidence

ORD record
ord-769402a7c83c4c97a813a448f0a25dad
Source dataset
uspto-grants-2000_08
Patent number
US06100260

Reaction notes

Loading…