Triethyl phosphite → 6-Diethylphosphono-2,2-dimethyl-2H-chromene
Reaction equation
Br[C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[O:8][C:7]([CH3:13])([CH3:12])[CH:6]=[CH:5]2.[P:14]([O:21]CC)([O:18][CH2:19][CH3:20])[O:15][CH2:16][CH3:17]>[Ni](Cl)Cl>[CH2:16]([O:15][P:14]([C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[O:8][C:7]([CH3:13])([CH3:12])[CH:6]=[CH:5]2)([O:18][CH2:19][CH3:20])=[O:21])[CH3:17]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 180 °C
Procedure
16 g of 6-bromo-2,2-dimethyl-2H-chromene are dissolved in 100 ml of triethyl phosphite. 2 g of nickel chloride are added and the mixture is refluxed at 180° C. for 24 hours in an autoclave. After the remaining triethyl phosphite has been concentrated, the expected product distills at 130°-140° C. under 0.1 mm Hg. 11.5 g are collected.
Workup
- concentrationAfter the remaining triethyl phosphite has been concentrated
- distillationthe expected product distills at 130°-140° C. under 0.1 mm Hg
- custom11.5 g are collected
Sources & evidence
- ORD record
- ord-33d77c441d1e4603a6b6341c3fc08971
- Source dataset
- uspto-grants-1995_02
- Patent number
- US05391751
Reaction notes
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