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Hydrochloric Acid → (R)-4-cyano-3-hydroxybutyric acid

HRID 2079451
Notes
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Reaction equation

HRID 2079451 reaction equation
[OH:1][CH:2](CC#N)[CH2:3][C:4]#[N:5].CC[O:11][C:12]([CH3:14])=[O:13].Cl>N#N>[OH:1][C@H:2]([CH2:3][C:4]#[N:5])[CH2:14][C:12]([OH:11])=[O:13]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 3617621,3-Dicyano-2-propanol

Product 1

HCID 10236005(R)-4-cyano-3-hydroxybutyric acid

Reagents, catalysts & solvents 1

HCID 947NitrogenSolvent

Procedure

3-hydroxyglutaronitrile (1 g, 9 mmol) was suspended in 37.5 mL of N2 (g) sparged, room temperature, 100 mM sodium phosphate buffer at pH 7. To this 240 mM solution of HGN was added 150 mg of cell lysate normalized for protein content. As assessed by PAGE, the nitrilase content was established to be 20% of the total protein. Therefore effectively, 30 mg of nitrilase is used in this reaction. The reaction was agitated at 100 rpm. Reaction progress was monitored by TLC (1:1 EtOAc:Hexanes, Rf=0.32, nitrile; Rf=0.0, acid) and GC. After 22 h, the reaction was filtered through a 10,000 MW cutoff filter and then concentrated in vacuo. The concentrated hydrolysis solution was acidified with 1M HCl and the product was continuously extracted with MTBE (30 mL). The acid product (R)-3-hydroxy-4-cyanobutyric acid was isolated as a yellow oil (1.15 g, 98% yield). 1H NMR (d6-DMSO, 500 MHz) δ12.32 (s, 1H), 5.52 (s, 1H), 4.10 (m, 1H), 2.70 (dd, 1H, J=16.8, 4.1 Hz), 2.61 (dd, 1H, J=16.9, 6.3 Hz), 2.44 (dd, 1H, J=15.4, 5.3 Hz), 2.37 (dd, 1H, J=15.6, 7.8 Hz). 13C NMR (DMSO, 298K, 125 MHz) δ171.9, 118.7, 63.4, 41.2, 25.2 MS calc'd for [C5H7NO3]: 129.0, found: 130.0 [M+H+], (ESI+). ee=95% [HPLC]. Based on the isolated yield a productivity of 40 g g−1 d−1 is calculated.

Workup

  1. customsparged, room temperature
  2. additionTo this 240 mM solution of HGN was added 150 mg of cell lysate
  3. customTherefore effectively, 30 mg of nitrilase is used in this reaction
  4. customReaction progress
  5. filtrationthe reaction was filtered through a 10,000 MW cutoff
  6. filtrationfilter
  7. concentrationconcentrated in vacuo
  8. customThe concentrated hydrolysis solution
  9. extractionthe product was continuously extracted with MTBE (30 mL)

Sources & evidence

ORD record
ord-ce68bc9b8b1343708d1a0c229c5a8f0f
Source dataset
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07932064B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes