Pyridine → HCID 22222978, compound

HRID 1744721Notes

Reaction equation

HRID 1744721 reaction equation
[CH:1]1([CH2:7][OH:8])[CH2:6][CH2:5][CH:4]=[CH:3][CH2:2]1.Cl[P:10]1(=[O:18])[O:15][CH2:14][C:13]([CH3:17])([CH3:16])[CH2:12][O:11]1.N1C=CC=CC=1>C(Cl)(Cl)Cl>[CH3:16][C:13]1([CH3:17])[CH2:14][O:15][P:10](=[O:18])([O:8][CH2:7][CH:1]2[CH2:6][CH2:5][CH2:4][CH:3]=[CH:2]2)[O:11][CH2:12]1

Participants

5

Reactant 3

HCID 1049PyridineHCID 155123-Cyclohexene-1-methanolHCID 777161,3,2-Dioxaphosphorinane, 2-chloro-5,5-dimethyl-, 2-oxide

Product 1

HCID 22222978HCID 22222978, compound

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

A 100 mL round bottom flask equipped with a stirrer bar was charged with 15.04 g (0.134 mol) 3-cyclohexene-1-methanol, 22.52 g (0.122 mol) of 2-chloro-5,5-dimethyl-1,3,2-dioxaphosphorinan-2-one, and 10.6 g (0.134 mol) of pyridine. After the above mixture was reacted at 80° C. for 3 hrs. The reaction mixture was added to chloroform (100 mL), and then washed with chloroform (2×100 mL), dried with sodium sulfate. The solvent was evaporated and the residue distilled to give pure product.

Workup

  1. customA 100 mL round bottom flask equipped with a stirrer bar
  2. customAfter the above mixture was reacted at 80° C. for 3 hrs
  3. washwashed with chloroform (2×100 mL)
  4. dry with materialdried with sodium sulfate
  5. customThe solvent was evaporated
  6. distillationthe residue distilled
  7. customto give pure product

Sources & evidence

ORD record
ord-6adecc57779c44f6ac523b9cafee511c
Source dataset
uspto-grants-2006_03
Patent number
US07018559B2

Reaction notes

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