3-Methyl-2-buten-1-OL → HCID 19369043, compound

HRID 848944Notes

Reaction equation

HRID 848944 reaction equation
[C:1](Cl)(=[O:5])[C:2]([Cl:4])=[O:3].[CH3:7][C:8]([CH3:12])=[CH:9][CH2:10][OH:11]>CCCCCCC>[C:2]([Cl:4])(=[O:3])[C:1]([O:11][CH2:10][CH:9]=[C:8]([CH3:12])[CH3:7])=[O:5]

Participants

4

Reactant 2

HCID 111733-Methyl-2-buten-1-OLHCID 65578Oxalyl chloride

Product 1

HCID 19369043HCID 19369043, compound

Reagents, catalysts & solvents 1

HCID 8900HeptaneSolvent

Procedure

A 1-liter eggplant type flask was charged with 25.4 g (0.20 mol) of oxalyl chloride and 250 ml of n-heptane, to which 21.5 (0.25 mol) of 3-methyl-2-buten-1-ol were added dropwise over 3 hours while bubbling nitrogen at room temperature, followed by stirring further for 2 hours. Thereafter, the reaction mixture was concentrated and distilled to obtain 11.6 g of 3-methyl-2-butenyl chlorooxalate.

Workup

  1. additionwere added dropwise over 3 hours
  2. customwhile bubbling nitrogen at room temperature
  3. concentrationThereafter, the reaction mixture was concentrated
  4. distillationdistilled

Sources & evidence

ORD record
ord-c5935296a37b4f30b2a308228945d52d
Source dataset
uspto-grants-2000_01
Patent number
US06010826

Reaction notes

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