SU489331A3 - Method for preparing 2,3-dihydro-1n-1,4-benzodiazepine derivatives - Google Patents

Description

1,4-bvneodiaeepina obteA formula

SaIb

b "- chSNg

 , n

Hat halogen atom, their salts,

licha shchi and sy so that soy overall formula 2

No1

where Hat is a helogen atom,

subjected to hydrolysis with an axes agent in the solvent.

The target product is recovered by a known technique in free form or in the form of its

salt.

Imidazolysinobeneophenone proiz -

aqueous general formula 2 can be obtained by reacting piperazine benzophenone derivative of general formula 3

Sbne

Hal

OH — where Hat is a halogen atom,

with acid in cfteee solvent.

For example, sodium, potassium, lithium, barium, calcium, ammonium, sodium carbonate, and potassium carbonate can be used as the base hydrolyzing agent.

In the quality of the solvent, it is advisable to use water, hydrogen, methanol, ethanol, 1trag dofuray.

The reaction proceeds at an elevated temperature, preferably at the boiling point of the solvent.

The benzodiazepine derivatives of formula 1 are converted to their corresponding salts by means of the treatment of the mineral kiggsgoy. such as hydrochloric, sulfuric, asotot or phosphose), or organic, for example, myleic, fumaric, amber, formic, acetic or oine.

The following benzodiazepine derivatives are obtained: 5-phenyl-2,3-digiaro-1H4, 4-benzodiaeepi11, 5 phenyl-7-chloro-2,3-dihydro-1H-1, 4-benzopyiazepine, 5-phenyl- in (or b) chloro-2,3-dihydr a-1H -1,4-benzoazazepine, 5-phenyl-7-bromo-2.3 digip |: o-1H-1, 4-benzodiazepine or their corresponding salts formed by hydrochloride , hydrobromic, phosphoric, succinic, fumaric, maleic acid. Example. 5-phenyl-7-chloro-2, 3-dihydro-1H-1, 4-beneodiazepine.

To a solution of 2 g of sodium hydroxide in 5 ml of water and 5 O ml of ethanol, add 3.3 g of 2- (2-oxo-azolysi1 {o) -5 "edl-benzophenone,

The reaction mixture was heated under reflux for 10 hours, then 50 ml of water was added and the mixture was filled. The mixture was heated under reflux for 17 of us, and the solvent fell to a supernatant at elevated pressure. The pot is washed with hot water and 2 g of a yellow solid are obtained, which is recrystallized from ethanol. 1.9 g of 5-phenyl-7-chloro -2,3-dihydro-1H-1,4-benzodiazepine are obtained; m.p. 173C; yield 67.5%.

Similarly, using the described procedure, but replacing the 2- (2-oxoimidazolysino) -5-hlarbenzophenone used in example 1 as the starting material, by 2- (2-oxonmidazylisino-5-bromobenzophenone, get 5-phenyl-7- € rum-2,3-digipro-111-., 4-b; nzoiazepine; mp 175-17 ° C.

Subject invention

Claims (4)

1. The method of obtaining the derivatives of 2,3-dihydro-1H-1,4-benzodiazene 1 by the general formula 1 where Hat is a halogen atom, or their salts with the selection of the target product in free form or as of its salt, characterized in that. that, in order to simplify the process and increase the yield of the target product, combine the general formula 2 Hatz - halogen atom. subjected to hydrolysis of the main agent, the volume in the environment of the solvent. 2. The method according to claim 1, about 7 liters, and with the fact that as the main agent using sodium hydroxide, potassium hydroxide, lithium hydroxide, barium hydrate, calpy hydroxide, ammonium hydroxide , sodium bicarone, potassium carbonate. 3. Method according to paragraphs. 1 and 2, distinguished by the fact that water, acetone, methanol, ethanol, tetrahytes | .K | fu1) an. 4. Method according to paragraphs. 1-3, which is carried out at the boiling point of the solvent.