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G.Patton

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Introduction

This method is presented the opportunity of Nitrazepam and 2-amino-5-nitrobenzophenone syntheses (also known as Mogadon; 7-nitro-5-phenyl-1,3-dihydro-1,4-benzodiazepin-2-one). There are two different ways of 2-amino-5-nitrobenzophenone, which have different precursors and levels of difficulty. Easiest way [1] has low yield, but doesn't take some manipulations and reagents. Another way takes some efforts but you'll get good yield. The final step of synthesis is Flash chromatography, which is so unlikable for underground low-skill chemists. Nevertheless, you can get the hang of it with help of BB forum manuals and complete this synthesis successfully.

Equipment and glassware:

  • 3 L and 1L three necked round bottom flasks;
  • Conventional funnel;
  • Filter paper;
  • Drip funnel;
  • CaCl2 drying tubes x2;
  • Heated magnetic stirrer;
  • Laboratory scale (0.01 — 100 g is suitable);
  • Beakers 1000 ml x2; 500 ml x2; 200 ml x2; 100 ml x2;
  • Glass rod;
  • 1 L Separating funnel;
  • pH Indicator stripes;
  • 2 L Buchner flask and funnel;
  • Laboratory grade thermometer (-10 — 250 °C);
  • 30 mm diameter column, 5 cm high column;
  • Silica gel (F254, Merck);
  • Water/ice bath;
  • Dean-Stark adapter/condenser.

Reagents:

  • 138 g (1 mole) 4-Nitroaniline;
  • 352 g (2.5 moles) Benzoyl choride;
  • 215 g (1.6 moles) Zinc chloride (ZnCl2);
  • ~2 L Distilled water;
  • 500 mL 75% (V/V) Sulfuric acid (H2SO4);
  • Ammonia aqueous solution (NH4OH);
  • 1 L 20 % Sodium hydroxide (NaOH);
  • Petroleum ether (+some benzene);
  • 1 L dry Pyridine [2];
  • 740 mL Toluene [2];
  • 350 mL Chloroform (CHCl3);
  • 24 mL (314 mmole) Chloroacetyl chloride;
  • 200 mL Tetrahydrofuran (THF);
  • 42 g (0.3 moles) Hexamine (hexamethylenetetramine);
  • 900 mL 96% Ethyl alcohol (EtOH);
  • 220 mL (2.95 moles NH3) 25% Ammonia solution, density 0.91 kg/L;
  • 1 g Toluenesulfonic acid hydrate;
  • 600 mL Dichloromethane (CH2Cl2).
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Boiling Point: 506.9 ± 60.0 °C at 760 mm Hg;
Melting Point: 226 - 229 °C;
Molecular Weight: 281.27 g/mole;
Density: 1.4 ± 0.1 g/ml (20 °C);
CAS Number: 146-22-5.

Procedures

2-Amino-5-nitrobenzophenone (2)
Method 1 [Low yield easy method]
The direct condensation in 3 L three necked round bottom flasks of 138 g (1 mole) 4-nitroaniline (1), 352 g (2.5 moles) benzoyl chloride and 215 g (1.6 moles) ZnCl2 at 200 °C for 2 h with reflux condenser, CaCl2 drying tube on the top of this condenser, magnetic/top stirring and thermometer (stirring, refluxing, moisture protection); hydrolysis after cooling down to r.t., washing out three times with boiling water (1 L) at 120 °C in separating funnel and hydrolysis of the brown-grey residue with 500 mL 75% (V/V) sulfuric acid in the 3 L three necked round bottom flasks with reflux condenser and thermometer for 40 min. at 140 °C (important or your product will decompose, concentration, time, temperature), after cooling down to r.t., partially neutralizing with ammonia (NH4OH) to pH 2 (!) gives a precipitate, which consists of 2-amino-5-nitrobenzophenone (2) and benzoic acid. This is stirred with 1 L 20% NaOH in the same three necked rb flasks for 3 h and suction filtered on a Buchner flask and funnel, then water-washed (2 L) in separating funnel and dried in rotary evaporator (vacuum, 80 °C). The product (2) m.p. 145 °C or is crystallized from petroleum ether (+some benzene). The yield is only 15% (calculated on nitroaniline!), 36 g.

NOTE: The Zinc Chloride mentioned in these syntheses is to be fresh and anhydrous, or it won't work.

Method 2 [A more complex method with a high yield]

Dissolve 138 g (1 mole) 4-nitroaniline (1) in 1 L dry pyridine in 3 L three necked round bottom flask with thermometer and add dropwise with ice-cooling - internal temp below 20 °C — 141 g (1.01 mole) benzoyl chloride over 2 h. Stir at 30 °C 24 h and evaporate to dryness at the rotavap in vacuo. Recover the expensive dist-off pyridine! The rest is suspended in 1 L 40 °C water and the product filtered and water-washed to remove pyridine rests. The mass is suspended in a 2 L flask in 500 mL toluene, a water-trap and a condenser are attached, and the mixture distilled to remove any water, then the toluene is distilled off in vacuo (recover) and then, it is dried at 80 °C in vacuo and weighed (weigh the flask before and after). The yield is about 242 g N-benzoyl-4-nitroaniline (2).
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2-(Сhloroacetamido)-5-nitrobenzophenone (3)
Dissolve 0.206 moles (50 g) 2-amino-5-nitrobenzophenone in 250 mL dry chloroform in 1 L two necked round bottom flask with thermometer, add over 5 min. 24 mL (314 mmole) chloroacetyl chloride, stir 2 h at 35 °C with moisture protection (CaCl2 tube). Evaporate all volatiles at the rotary evaporator, add more 100 mL chloroform to the residue and evaporate again to total dryness.
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7-nitro-5-phenyl-1,3-dihydro-1,4-benzodiazepin-2-one (Nitrazepam) (4)
Take up the resultant 2-(chloroacetamido)-5-nitrobenzophenone (3) in 200 mL THF, add 42 g (0.3 moles) Hexamine (hexamethylenetetramine), 900 mL 96% alcohol, and 220 mL (2.95 moles NH3) 25% ammonia solution, density 0.91 kg/L in 3 L three necked round bottom flasks with thermometer and reflux condenser. Reflux for 6 hrs, evaporate (rest in vacuo at the rotary evaporator) all volatiles, add 240 mL toluene and 1 g toluenesulfonic acid hydrate and shake. Reflux with Dean-Stark adapter/condenser in them for 90 min., add 150 mL hot water and let cool down overnight. Filter of the brown solid, wash twice with 100 mL water in separating funnel and dissolve in 400 mL dichloromethane.
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