Triethylamine → HCID 66855304, compound

HRID 1970501Notes

Reaction equation

[N:1]1([C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.C(N(CC)CC)C.[CH2:21]([O:25][C:26](Cl)=[O:27])[CH2:22][CH2:23][CH3:24]>ClCCl>[C:10]([O:9][C:7]([N:1]1[CH2:6][CH2:5][N:4]([C:26]([O:25][CH2:21][CH2:22][CH2:23][CH3:24])=[O:27])[CH2:3][CH2:2]1)=[O:8])([CH3:13])([CH3:12])[CH3:11]

Participants

Conditions

Temperature: 0 °C

Procedure

To a solution of 10.9 g tert-butyl 1-piperazinecarboxylate in 145 ml dichloromethane were added 17.8 ml triethylamine. The solution was cooled to 0° C. and 8.3 ml butylchloro-formate added dropwise at this temperature. After stirring for 1 h the reaction mixture was diluted with dichloromethane and washed with 0.1 M HCl and saturated NaHCO3. The crude product obtained after evaporation of the solvent was directly used in the next reaction step. Yield: 18.0 g.

Workup

washwashed with 0.1 M HCl and saturated NaHCO3

Sources & evidence

ORD record: ord-4f9058b2111546c89214bbdd74215cf1
Source dataset: uspto-grants-2013_04
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US08426420B2

Reaction notes

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