ChemicalBook CAS DataBase List 1,2,3,4-tetrahydrobenzo(e)(1,4)diazepin-5-one

1,2,3,4-tetrahydrobenzo(e)(1,4)diazepin-5-one synthesis

7synthesis methods

Product Name:1,2,3,4-tetrahydrobenzo(e)(1,4)diazepin-5-one
CAS Number:28544-83-4
Molecular formula:C9H10N2O
Molecular Weight:162.19

610-96-8
245 suppliers
$10.00/5g

107-15-3
9 suppliers
$11.19/25ML

1,2,3,4-tetrahydrobenzo(e)(1,4)diazepin-5-one

28544-83-4
50 suppliers
$17.00/100mg

Yield:28544-83-4 52.6%

Reaction Conditions:

with potassium carbonate in N,N-dimethyl-formamide;Inert atmosphere;

Steps:

1.A Step A: 1,2,3,4-tetrahydro-5H-benzo[e][1,4]diazepin-5-one

Under N2 protection,Methyl 2-chlorobenzoate (5.00 g, 0.029 mol),Ethylenediamine(8.81 g, 0.15 mol) and anhydrous potassium carbonate (8.10 g, 0.59 mol) in DMF (100 mL)cool down,Concentrated under reduced pressure,Add water to the residue,Extract three times with ethyl acetate.Combine the ethyl acetate phase,Wash with saturated sodium chloride solution,Dry anhydrous sodium sulfate,Concentration gave a black residue.Chromatography of the residue on silica gel eluting with ethyl acetate / petroleum ether gradient(20-50%) elution,getWhite solid product (2.5 g, 52.6%).

References:

CN108498520,2018,A Location in patent:Paragraph 0025; 0027; 0028; 0029; 0030