Preparation of diazomethane a dilute ethereal solution

The set-up shown in Fig. 6,21 can be used to prepare between 3 and 17raraol of diazomethane. 

Dissolve potassium hydroxide (Ig) in water (2ml), dilute with 95% ethanol (8ml), and add to the reaction flask. Cool the flask in an ice bath, then slowly add a solution of Diazald (iV-raethyl-N-nitroso-p-toluenesuphonamide) in diethyl ether (15ml), using a Pasteur pipette. When all the Diazald (Ig) has been added, stopper the neck of the flask, put the ice bath under the receiver and place a warm water bath (about bS C) under the reaction flask. The yellow diazomethane-ether mixture will start to distil out of the flask. Carry-on distilling until all the yellow colour has disappeared from the reaction flask, adding a further 5ml of diethyl ether if necessary. The yellow distillate contains diazomethane (about 3.3mmol). 

To produce diazomethane (16.6mmol) use Diazald (5g), potassium hydroxide (5g), water (8ml), ethanol (10ml) and diethyl ether (50ml). The 

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