Diazomethane → HCID 54486441, compound

HRID 972277Notes

Reaction equation

HRID 972277 reaction equation
[CH:1]1([CH2:7][C:8](Cl)=[O:9])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[N+:11](=[CH2:13])=[N-:12]>CCOCC>[N+:11](=[CH:13][C:8]([CH2:7][CH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1)=[O:9])=[N-:12]

Participants

4

Reactant 2

HCID 9550DiazomethaneHCID 2757989Cyclohexylacetyl chloride

Product 1

HCID 54486441HCID 54486441, compound

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent2×

Procedure

A solution of 19.8 g of cyclohexylacetyl chloride (b.p. 98° - 100°/23 mm Hg) in 150 ml of dry ether is slowly added at 0°-5° with cooling in an ice-water bath to a vigorously stirred solution of 11 g of diazomethane in 500 ml of ether. The excess diazomethane and ether is distilled off under reduced pressure and cyclohexylmethyl diazomethyl ketone is obtained as residue; infra-red absorption spectrum (in methylene chloride): characteristic bands at 3.45μ, 3.52μ, 4.75μ and 6.12μ; the product is processed without any further purification.

Workup

  1. distillationThe excess diazomethane and ether is distilled off under reduced pressure

Sources & evidence

ORD record
ord-5fc8cf98eb96412287556abac7d6bebb
Source dataset
uspto-grants-1977_10
Patent number
US04052408

Reaction notes

Loading…