Thionyl Chloride → HCID 21568326, compound
Reaction equation
[OH:1][P:2]1(=O)[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH2:5][CH2:4][CH2:3]1.S(Cl)([Cl:15])=O>>[Cl:15][P:2]1(=[O:1])[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH2:5][CH2:4][CH2:3]1Participants
3
Procedure
1-Hydroxy-1-oxo-1,2,3,4-tetrahydrophosphinoline (2.7g, 15 mmole) was refluxed with redistilled thionyl chloride (12 ml, 170 mmole) for 2 hr, and the excess of thionyl chloride removed by distillation. Distillation of the residue (bulb to bulb) at 150°/0.005 mm gave 1-chloro-1-oxo-1,2,3,4-tetrahydrophosphinoline (34), a light yellow fuming solid (2.3g, 76%). This was used without further purification.
Workup
- customthe excess of thionyl chloride removed by distillation
- distillationDistillation of the residue (bulb to bulb) at 150°/0.005 mm
Sources & evidence
- ORD record
- ord-0ba3dad72bfc437da1c7dae8565abb5d
- Source dataset
- uspto-grants-1976_01
- Patent number
- US03931196
Reaction notes
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