Organometallics · Section 98 of 116

Grignard reagents

Practice this — interactive lesson

A Grignard reagent is made by stirring an alkyl, vinyl or aryl halide with magnesium turnings in dry ether. The metal inserts into the carbon–halogen bond:

R–Br + Mg → R–MgBr

Nothing is added and nothing leaves. The same carbon that was δ+ in the halide comes out δ− in the product, which is the polarity reversal the previous section described.

Why the solvent has to be ether

Diethyl ether or THF is not incidental. The magnesium of a Grignard is electron-poor, and the two lone pairs on the ether oxygen coordinate to it, which is what keeps the reagent in solution and stable enough to use. Try the same reaction in a hydrocarbon and it does not work; try it in anything with an O–H and the reagent destroys the solvent.

Dry means dry. Traces of water quench the reagent as fast as it forms, and the usual symptom of a failed Grignard is not a mess but simply nothing happening — the halide sits there and the magnesium never gets consumed.

What a Grignard attacks

The mechanism is always the same: the nucleophilic carbon attacks an electrophilic carbon, and an acidic workup protonates whatever anion is left. What differs is the electrophile, and the products are worth learning as a set, because the carbon count changes differently in each case.

ElectrophileProduct after H3O+Carbons gained
Formaldehyde, HCHOPrimary alcoholone
Any other aldehydeSecondary alcoholtwo or more
KetoneTertiary alcoholthree or more
Carbon dioxideCarboxylic acidone
Epoxide (at the less hindered carbon)Alcohol, further along the chaintwo, for ethylene oxide
Nitrile, then hydrolysisKetoneone plus the R group
Ester or acyl chlorideTertiary alcohol, two R groups addedsee below

The one-carbon extensions are the three worth memorizing together, because each ends somewhere different: formaldehyde gives a primary alcohol, CO2 gives a carboxylic acid, and a nitrile gives a ketone. Asked to lengthen a chain by exactly one carbon, you pick from that list according to what functional group you want at the end.

The ester problem

electrophilecarbon groups already thereproductFormaldehyde0 C groups1° alcoholOther aldehyde1 C group2° alcoholKetone2 C groups3° alcoholEster1 C group, but adds twice3° alcoholThree of these are a counting exercise. The fourth needs a mechanism:the ester expels alkoxide to a ketone that is hungrier than the ester was.
What comes out of a Grignard addition, sorted by how many carbon groups the electrophile already carried. Formaldehyde has none and gives a primary alcohol, any other aldehyde has one and gives a secondary, a ketone has two and gives a tertiary.The ester is the row that breaks the pattern, and it is the one people get wrong. It starts with one carbon group like an aldehyde, but the first addition expels the alkoxide to leave a ketone — and a ketone has no electron-donating OR group, so it is a better electrophile than the ester was. A second equivalent attacks before you can stop it, which is why limiting the stoichiometry does not help.

An ester looks like a way to make a ketone, and it is not. The Grignard adds once, the tetrahedral intermediate collapses by expelling the alkoxide, and what is left is a ketone that is more electrophilic than the ester was. The second equivalent of Grignard attacks it immediately.

So the product is a tertiary alcohol carrying two identical R groups from the Grignard, and stopping at the ketone by using one equivalent does not work — the ketone is consumed faster than it forms. An acyl chloride ends up in the same place by a different route. It is the most electrophilic acyl derivative, so the ester argument does not transfer — the ketone it gives is less reactive than the acyl chloride was. It is still reactive enough to be attacked as fast as it forms, which is enough to spoil the selectivity.

If you actually want the ketone, you need a reagent that is not reactive enough to add twice. A Gilman reagent stops after one addition to an acyl chloride; a Weinreb amide holds the first intermediate as a stable chelate until workup. Both are answers to this specific failure.

Grignards as bases, which is usually the problem

Every one of the reactions above assumes the substrate has no acidic hydrogen. Put an alcohol, a carboxylic acid, an amine, a thiol or a terminal alkyne anywhere in the molecule and the Grignard removes that proton instead, giving R–H and a magnesium salt. The reagent is consumed and the carbonyl is untouched.

Three routes around it, in the order you should consider them:

What carries forward

A Grignard is nucleophilic carbon that adds once to an aldehyde or ketone and twice to an ester, gives a primary, secondary or tertiary alcohol depending on what it hit, and is destroyed by any acidic proton in the flask. When a route needs a C–C bond next to an oxygen, this is almost always the reaction — and when a route on paper does not work in practice, an acidic hydrogen is almost always the reason.