3-methylpentanoyl chloride

Conditions: temp:-7.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To commercially available biphenyl (0.08 mole) and anhydrous aluminium trichloride (0.1 mole) dissolved in dry nitrobenzene (90ml), (+)-3-methylpentanoylchloride (0.1mole) the preparation of which is known and described in United Kingdom Patent Application No. 36211/75), is added in drops, the temperature being maintained at about -7° C. during the addition. The mixture is then stirred for about 18 hr. with cooling in an ice bath. It is then poured onto a mixture of ice, water and concentrated hydrochloric acid and stirred for 0.5 hr., and the nitrobenzene layer is separated. The nitrobenzene is removed by steam distillation and the residue is crystallised from a small volume of ethanol to constant melting point. 36211/75), is added in drops with cooling in an ice bath stirred for 0.5 hr , and the nitrobenzene layer is separated The nitrobenzene is removed by steam distillation the residue is crystallised from a small volume of ethanol to constant melting point

Conditions: temp:-7.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To commercially available biphenyl (0.08 mole) and anhydrous aluminium trichloride (0.1 mole) dissolved in dry nitrobenzene (90ml), (+)-3-methylpentanoylchloride (0.1mole) the preparation of which is known and described in United Kingdom Patent Application No. 36211/75), is added in drops, the temperature being maintained at about -7° C. during the addition. The mixture is then stirred for about 18 hr. with cooling in an ice bath. It is then poured onto a mixture of ice, water and concentrated hydrochloric acid and stirred for 0.5 hr., and the nitrobenzene layer is separated. The nitrobenzene is removed by steam distillation and the residue is crystallised from a small volume of ethanol to constant melting point. 36211/75), is added in drops with cooling in an ice bath stirred for 0.5 hr , and the nitrobenzene layer is separated The nitrobenzene is removed by steam distillation the residue is crystallised from a small volume of ethanol to constant melting point

Conditions: temp:-7.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To commercially available biphenyl (0.08 mole) and anhydrous aluminium trichloride (0.1 mole) dissolved in dry nitrobenzene (90ml), (+)-3-methylpentanoylchloride (0.1mole) the preparation of which is known and described in United Kingdom Patent Application No. 36211/75), is added in drops, the temperature being maintained at about -7° C. during the addition. The mixture is then stirred for about 18 hr. with cooling in an ice bath. It is then poured onto a mixture of ice, water and concentrated hydrochloric acid and stirred for 0.5 hr., and the nitrobenzene layer is separated. The nitrobenzene is removed by steam distillation and the residue is crystallised from a small volume of ethanol to constant melting point. 36211/75), is added in drops with cooling in an ice bath stirred for 0.5 hr , and the nitrobenzene layer is separated The nitrobenzene is removed by steam distillation the residue is crystallised from a small volume of ethanol to constant melting point

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A solution of 1.2 g (0.005 mole) of 2,4,2',4'-tetrahydroxybenzophenone and 3 g (0.025 mole) of 3-methyl valeroylchloride was warmed to 50° C. for 4 hrs. in 50 mls of dry pyridine. Solvent removal via rotary evaporator left an oil. This was partitioned between H2O and CH2Cl2. The organic layer was washed with K2CO3 solution (5%) and dried over MgSO4. After filtration and solvent removal the product remained an oil; 2.5 g (78%) yield. Solvent removal via rotary evaporator left an oil This was partitioned between H2O and CH2Cl2 The organic layer was washed with K2CO3 solution (5%) dried over MgSO4 After filtration and solvent removal the product 2.5 g (78%) yield

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A solution of 1.2 g (0.005 mole) of 2,4,2',4'-tetrahydroxybenzophenone and 3 g (0.025 mole) of 3-methyl valeroylchloride was warmed to 50° C. for 4 hrs. in 50 mls of dry pyridine. Solvent removal via rotary evaporator left an oil. This was partitioned between H2O and CH2Cl2. The organic layer was washed with K2CO3 solution (5%) and dried over MgSO4. After filtration and solvent removal the product remained an oil; 2.5 g (78%) yield. Solvent removal via rotary evaporator left an oil This was partitioned between H2O and CH2Cl2 The organic layer was washed with K2CO3 solution (5%) dried over MgSO4 After filtration and solvent removal the product 2.5 g (78%) yield