Nooglutyl → 2365144-97-2

HRID 1661881Notes

Reaction equation

HRID 1661881 reaction equation
[OH:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([CH:19]=1)[C:7]([NH:9][C@H:10]([C:16]([OH:18])=[O:17])[CH2:11][CH2:12][C:13]([OH:15])=[O:14])=[O:8].[O-2].[Ca+2:21]>O>[OH:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([CH:19]=1)[C:7]([NH:9][C@H:10]([C:16]([O-:18])=[O:17])[CH2:11][CH2:12][C:13]([O-:15])=[O:14])=[O:8].[Ca+2:21]

Participants

4

Reactant 2

HCID 147523NooglutylHCID 6850728Calciumoxide

Product 1

HCID 866346012365144-97-2

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

Heat suspension of 2.68 g (0.01M) of N-(5-hydroxynicotinoyl)-L-glutamic acid in 50 ml of water up to 60-70° C. and add 0.68 g (0.012M) of calcium oxide in small portions. The sediment gradually dissolves. Heat the suspension for complete dissolution. Evaporate aquatic solution to 20 ml. Add resultant solution dropwise to 200 ml of ethanol. Mix formed precipitate for 0.5 hour and leave it for 12 hours at room temperature. Filter the precipitate, wash with alcohol and dry at 100° C. for constant weight (3 hours). Calcium N-(5-hydroxynicotinoyl)-L-glutamate (I) is obtained, recovery is 2.7 g (83%), [α]D20+11° (c 1, water).

Workup

  1. temperatureHeat
  2. dissolutionThe sediment gradually dissolves
  3. temperatureHeat the suspension
  4. dissolutionfor complete dissolution
  5. customEvaporate aquatic solution to 20 ml
  6. additionAdd resultant solution dropwise to 200 ml of ethanol
  7. additionMix
  8. customformed precipitate for 0.5 hour
  9. customleave it for 12 hours at room temperature
  10. filtrationFilter the precipitate
  11. washwash with alcohol
  12. customdry at 100° C. for constant weight (3 hours)

Sources & evidence

ORD record
ord-bacc63bfafac4063bfedc80f922cabda
Source dataset
uspto-grants-2011_10
Patent number
US08030493B2

Reaction notes

Loading…