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ChemicalBook CAS DataBase List FMOC-LYS(BOC)(ME)-OH

FMOC-LYS(BOC)(ME)-OH synthesis

7synthesis methods
24424-99-5 Synthesis
Di-tert-butyl dicarbonate

24424-99-5
823 suppliers
$13.50/25G

Benzenebutanamide, N-8-quinolinyl-

1449300-08-6
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Yield:951695-85-5 224 g

Reaction Conditions:

with sodium hydrogencarbonate in tetrahydrofuran;water at 20; for 4 h;Reagent/catalyst;

Steps:

1-5

Use the above pale yellow solid crude product 1: 1 of water (500 mL) and THF (500 mL) dissolved, Add sodium bicarbonate (63 g, 0.75 mol), Stir until clarified, (Boc) 2O (142 g, 0.65 mol) in tetrahydrofuran (200 mL), Room temperature reaction 4.0h, HPLC detection showed complete reaction of the starting material. The reaction solution is neutralized with alkene hydrochloride to a pH of 5-6. The organic solvent was removed by concentration under reduced pressure. The aqueous phase was extracted with ethyl acetate. Washed with saturated saline, The organic phase was concentrated to give a white solid product (235 g). The white solid was recrystallized from ethyl acetate and n-hexane. Obtained 224 g of a white solid powder. The yield was 93% and the purity was 99.8%.

References:

CN108383757,2018,A Location in patent:Paragraph 0019; 0028; 0029; 0033; 0034; 0038; 0039; 0043

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