For the synthesis of L-lyxose-5-phosphates 11a-13a (Scheme 4A) the ATP recycling system was omitted since the PEP based inhibition of TIM was not needed for L-G3P. Reactions were instead carried out at 20 mM substrate loading with stoichiometric amounts of ATP. The initial substrate chosen to analyse was the 2-OMe, due to its diagnostic singlet peak in 1 H NMR. Conditions for the scaleup reaction of L-lyxose-5-phosphates were optimized via design of experiment (DOE) (supplementary 11.2.1). The most significant factors were found to be both aldolase and donor substrate concentrations.