Organometallics · Section 99 of 116

Organolithiums and acetylides

Practice this — interactive lesson

An organolithium is made the same way a Grignard is — a halide plus the metal, in a dry ether or hydrocarbon solvent — except that it takes two equivalents of lithium, because each lithium carries one electron and one of them leaves as LiBr:

R–Br + 2 Li → R–Li + LiBr

Everything a Grignard does, an organolithium also does. The reason to reach for one is that lithium is more electropositive than magnesium, so the carbon carries more negative charge, and the reagent is both a stronger nucleophile and a stronger base. Sometimes that extra reactivity is what you need; more often it is what you have to manage.

Where RLi succeeds and RMgX does not

Two cases come up repeatedly.

A hindered ketone. A Grignard approaching a very crowded carbonyl often gives enolization — it acts as a base on the α hydrogen instead of adding — or reduction by hydride transfer from its own β carbon. An organolithium, being smaller and more reactive, adds cleanly where the Grignard stalls.

A carboxylic acid straight to a ketone. This one looks impossible. A carboxylic acid has an O–H, so the first equivalent of RLi is spent deprotonating it. But the carboxylate that results is a poor electrophile with a full negative charge, and an organolithium is reactive enough to add to it anyway, giving a doubly charged intermediate that cannot collapse. Collapsing would mean expelling O²⁻, which is no leaving group at all, and would pile a third negative charge onto a center that already carries two. So it sits there until the acidic workup, and only then does it lose water to give the ketone.

The dianion is why the reaction stops at the ketone. Nothing protects the ketone from a second addition — the ketone does not exist until workup, by which point the organolithium is gone. Compare this with the ester case, where the ketone does form in the flask and gets attacked at once. Two equivalents of RLi are needed, one for the proton and one for the addition.

Deprotonation as the goal

from an esterCOORR′Rfrom RLicollapses in the flaskthe ketone forms, and is attacked againfrom a carboxylateCOORR′from RLicannot collapse — two chargesthe ketone appears only on workupNothing protects the ketone in the second case. There is no ketone to protectuntil the reagent has already been used up.
Why RLi takes a carboxylic acid to a ketone and stops, while a Grignard takes an ester past one. Both add to a carbonyl and both give a tetrahedral intermediate. The ester’s has an alkoxide to expel, so it collapses at once; the carboxylate’s is a dianion, and expelling anything from it would mean pushing charge onto an already charged center.Two equivalents of RLi are needed here, and they do different jobs: the first is spent taking the acidic O–H proton, and only the second adds. The organolithium is doing something a Grignard cannot, which is attacking a carbonyl that already carries a full negative charge.

Because RLi reagents are extremely strong bases, several of the ones you will meet exist to remove a proton rather than to form a C–C bond:

ReagentUsed for
n-BuLiGeneral-purpose strong base; deprotonating terminal alkynes and heteroaromatics
t-BuLiThe same but far more so; also the standard reagent for lithium–halogen exchange
LDA (from n-BuLi and diisopropylamine)The classic enolate base: very strong, too bulky to add to a carbonyl

LDA is the one worth tracing back. It is made by using n-BuLi as a base on an amine, and its whole point is the combination it achieves: strong enough to deprotonate a ketone completely, yet too hindered to attack the carbonyl. That pairing of high basicity with low nucleophilicity is not something a Grignard can offer, and it is what makes controlled enolate chemistry possible.

Acetylides, the cheapest carbon nucleophile

A terminal alkyne has a pKa of about 25 — acidic for a C–H, because the carbanion sits in an sp orbital with high s character. NaNH2 or n-BuLi removes that proton to give an acetylide, which is a genuine carbon nucleophile made without any transition metal.

An acetylide will do SN2 on a methyl or primary halide, and it adds to aldehydes and ketones. The SN2 is the useful half, and it is worth noting that an ordinary sp³ organometallic and an alkyl halide do not generally do this, because elimination and self-coupling get there first. The contrast is between an sp carbanion and an sp³ one rather than between reagent families — an acetylide is often a magnesium or lithium salt itself.

Do not push it. With a secondary or tertiary halide the acetylide is basic enough that E2 wins and you get an alkene instead of the coupled product. Primary or methyl only.

What carries forward

An organolithium is a Grignard with the volume turned up: same reactions, more reactivity, less selectivity. Use it where a Grignard stalls on a hindered ketone or where you want a ketone from a carboxylic acid, and recognize it in its other role as the base behind LDA and the acetylides. The next section goes the opposite way and turns the reactivity down, which turns out to buy more than turning it up ever does.