HCID 21478646, compound → HCID 21478575, compound

HRID 2292510Notes

Reaction equation

HRID 2292510 reaction equation
CO[CH2:3][CH2:4][CH2:5][N:6]1[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=2[NH:10][C:9](=[O:17])[CH2:8][C:7]1=[O:18].[BrH:19].C(O)(=O)C>O>[Br:19][CH2:3][CH2:4][CH2:5][N:6]1[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=2[NH:10][C:9](=[O:17])[CH2:8][C:7]1=[O:18]

Participants

4

Reactant 2

HCID 21478646HCID 21478646, compoundHCID 21893785Acetic Acid Mixture with Hydrobromic Acid

Product 1

HCID 21478575HCID 21478575, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
60 °C

Procedure

To 4.9 g of the compound of Example 208, 25 ml of 30% hydrobromic acid-acetic acid solution is added and the resulting mixture is stirred at 60° C. for 4.7 hours. The resulting mixture is poured into water and the resultant is subjected to extraction with ethyl acetate. The organic layer is washed with aqueous sodium carbonate solution and brine and dried. The resultant is purified by silica gel column chromatography (ethyl acetate) to obtain 3.3 g of (209).

Workup

  1. extractionthe resultant is subjected to extraction with ethyl acetate
  2. washThe organic layer is washed with aqueous sodium carbonate solution and brine
  3. customdried
  4. customThe resultant is purified by silica gel column chromatography (ethyl acetate)

Sources & evidence

ORD record
ord-28b831defe1d4b918847e2f462cf04c2
Source dataset
uspto-grants-1997_11
Patent number
US05683998

Reaction notes

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