ALDRICH(R) DIAZOMETHANE-GENERATOR WITH SYSTEM 45(R) COMPATIBLE CONNECTION

General description

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.

Note: We are unable to supply certain Diazomethane precursors in some countries. Check availability of starting materials prior to glassware purchase.

Typical Generator Procedure:
To the outside tube of the Aldrich MNNG diazomethane generation apparatus, add 4-methoxybenzoic acid (0.0465 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 (0.0490 g, 0.295 mmol, 98.4%). Analysis by GC/MS indicates the material to be analytically pure.

Replacement parts:
Z411744 O-ring seal
Z411760 PTFE-faced silicone septum, 8 mm
Z411779 Screw-cap with hole, 8 mm
Z230723 Disposable PE/PP syringes, 1 mL
Z412139 Disposable 22 gauge needles, 1 in. L

Call or visit our website for pricing on replacement parts.
For technical and safety information about Diazald and Aldrich diazomethane generators see Technical Information Bulletin AL-180.

Legal Information

Aldrich is a registered trademark of Sigma-Aldrich Co. LLC

System 45 is a trademark of John Babashak