Aldrich^® diazomethane-generator with System 45^® compatible connection 

This apparatus incorporates a System 45 screw-thread connection that eliminates glass joints, clamps, and grease and permits the preparation of diazomethane without the need for codistillation with ether (see below). Request Technical Information Bulletin No. AL-180.
The screw-thread closure and PTFE adapter provide an efficient, gas tight connection between the inner tube and the outer body section. For storage, simply remove the inner tube assembly from the threaded outer section and screw on the PTFE lined screw cap. Access to the material may be made through the open top septum cap with a syringe. Supplied complete with threaded body, threaded inner tube, PTFE adapter, 32 mm cap, O-ring, lock nut, septum and 8 mm open top cap.

Typical Generator Procedure
To the outside tube of the Aldrich MNNG diazomethane generation apparatus, add 4-methoxybenzoic acid (0.465 g, 0.300 mmol) and ether (3.0 mL). To the inside tube, add Diazald (0.367 g, 1.71 mmol) and carbitol (1.0 mL). Assemble the two parts and immerse the lower part of the outer tube in an ice bath. After equilibrating to the cooling bath temperature, Slowly inject, dropwise through the septum via a syringe, aqueous KOH (37%, ~1.5 mL). Shake the apparatus gently by hand to ensure mixing of reactants within the inner tube, while being careful not to allow these reactants to spill into the outer tube. The solution in the outer tube may became yellow in color and will persisted, indicating an excess of diazomethane. After 50 min, open the apparatus. Carefully add solid silicic acid (0.151 g) to the inner tube to destroy unreacted diazomethane. Evaporate the yellow ether solution in the outside tube under a gentle stream of nitrogen affording methyl 4-methoxybenoate as a white solid product (0.490 g, 98.4%). Analysis by GC/MS indicates the material to be analytically pure.

Replacement parts:
Z41,174-4 O-ring seal
Z41,176-0 PTFE-faced silicone septum, 8 mm
Z41,177-9 Screw-cap with hole, 8 mm
Z23,072-3 Disposable PE/PP syringes, 1 mL
Z41,213-9 Disposable 22 gauge needles, 1 in. L

Call or visit our website for pricing on replacement parts.

System 45 is a registered trademark of NDS Technologies, Inc.