Ammonia → HCID 23615384, compound

HRID 1065996Notes

Reaction equation

HRID 1065996 reaction equation
C([O-])=O.[NH4+].[Na+].O=[C:7]([C:11]([CH3:15])([CH3:14])[CH2:12][CH3:13])[C:8]([O-:10])=[O:9].N.C1[N:18]=C(N)C2N=CN([C@@H]3O[C@H](COP(OP(OC[C@H]4O[C@@H](N5C=C(C(N)=O)CC=C5)[C@H](O)[C@@H]4O)(O)=O)(O)=O)[C@@H](O)[C@H]3O)C=2N=1.N[C@H](C(O)=O)CC(C)C.C([O-])=O.C>O>[CH3:14][C:11]([CH2:12][CH3:13])([CH3:15])[C@@H:7]([C:8]([OH:10])=[O:9])[NH2:18]

Participants

9

Reactant 7

HCID 222Ammonia2×HCID 283FormateHCID 297MethaneHCID 6106L-LeucineHCID 439153NadhHCID 2723923Ammonium formateHCID 88230955HCID 88230955, compound

Product 1

HCID 23615384HCID 23615384, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

6.3 g (0.1 mole) ammonium formate and 1.67 g (10 mmoles), 2-keto-3,3-dimethyl pentanoic acid sodium salt are suspended in 80 ml of water, the pH value is adjusted with ammonia to 8.2, so that the solids dissolve and the volume is adjusted to 100 ml. subsequently, 14.34 mg (0.02 mmole) NAD+3H2O cofactor as well as 800 U of leucine dehydrogenase (LeUDH) and 500 U of rec-formate dehydrogenase (rec-FDH) are added. The temperature is set to 32° C . During the reaction the system is gently stirred and the pH value is adjusted to 8.2 via a pH stat unit. The completion point of the reaction is sdemonstrated by determining the degree of conversion with HPLC. The reaction solution is adjusted to pH 9,5 with ammonia and subsequently clarified with 2% active charcoal. The almost colourless solution is concentrated with a rotary evaporator, the amino acid is crystallized, is separated via a filter funnel, washed three times with a little ethanol and dried overnight under vacuum at 50° C.

Workup

  1. dissolutiondissolve
  2. customis set to 32° C
  3. customDuring the reaction the system
  4. concentrationThe almost colourless solution is concentrated with a rotary evaporator
  5. customthe amino acid is crystallized
  6. customis separated via a filter funnel
  7. washwashed three times with a little ethanol
  8. customdried overnight under vacuum at 50° C.

Sources & evidence

ORD record
ord-1477ca8f411f459f8d94a9d9564cdca0
Source dataset
uspto-grants-2001_06
Patent number
US06242234B1

Reaction notes

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