Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | HCID 20443377 | HCID 20443377 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 54450268 | HCID 54450268 | — |
Reaction Steps
15 g of para-formaldehyde are added, at 70°C and with vigorous agitation, to 100 g (0.505 mole) of benzenephosphonous acid isobutyl ester. Agitation is continued for 1 hour at 75°-90°C. The reaction mixture is then cooled, stirred with water, and the organic phase is separated. The aqueous phase is extracted 2 times with chloroform, and the extract is added to the organic phase. After drying with sodium sulfate, distillation is carried out in a water jet vacuum at an interior temperature of up to 80°C. The residue is distilled in a thin layer evaporator at 0.1 torr and a distillation temperature of 190°C. Subsequently, the distillate is again distilled in a normal distillation apparatus. It is pure hydroxymethyl-phenylphosphinic acid isobutyl ester having a boiling point of 155°C at 0.3 torr.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US03943170 |
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| Source dataset | uspto-grants-1976_03 |
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| ORD ID | ord-18c52abc51f24f5d921c7195fdab4a03 |
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| Source note | uspto-grants-1976_03 |
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