N-TERT-BUTYL-N'-METHYL ETHYLENEDIAMINE synthesis

Yield:89893-79-8 1.5 g

Reaction Conditions:

with sodium tris(acetoxy)borohydride;acetic acid in chloroform at 20;

Steps:

16 First step: 4-(tetrahydro-2H-pyran-4-yl)piperazine-1-carboxylic acid tert-butyl ester

General procedure: Piperazine-1-carboxylic acid tert-butyl ester (1.0 g, 5.37 mmol) was sequentially added to a 100 mL single-mouth bottle.Tetrahydro-4H-pyran-4-one (1.07g, 10.7mmol) and methanol (20mL), sodium cyanoborohydride (507mg, 8.06mmol) was added in portions, added, 0.5mL acetic acid was added, and the reaction was stirred at room temperature. 6-7h.The reaction was monitored by TLC. After completion of the reaction, the reaction was quenched with EtOAc EtOAc (EtOAc) The crude product was purified by column chromatography.Elution with DCM/MeOH = 20/1, product was collected and concentrated.1.5 g of a colorless oil were obtained.

References:

CN108707139,2018,A Location in patent:Paragraph 0253; 0255; 0259; 0260; 0261; 0262