http://rdf.ncbi.nlm.nih.gov/pubchem/patent/GB-565452-A
Outgoing Links
| Predicate | Object |
|---|---|
| assignee | http://rdf.ncbi.nlm.nih.gov/pubchem/patentassignee/MD5_6b99b6943a51b3e4e6eef221a17d90ee |
| classificationCPCInventive | http://rdf.ncbi.nlm.nih.gov/pubchem/patentcpc/C07D307-10 http://rdf.ncbi.nlm.nih.gov/pubchem/patentcpc/C07C17-16 |
| classificationIPCInventive | http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07C17-16 http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07D307-10 |
| filingDate | 1944-01-06-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
| publicationDate | 1944-11-10-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
| publicationNumber | GB-565452-A |
| titleOfInvention | Improvements in the manufacture of iodides and bromides from alcohols |
| abstract | <PICT:0565452/IV/1> Iodides of normal or branched chain, primary or secondary alcohols, are prepared by heating a mixture of the alcohol and red phosphorus in a main reaction vessel so that the alcohol boils and passes into a subsidiary vessel containing the iodine which dissolves in the hot alcohol, which in the case of the lower alcohols is near its boiling point, the solution being returned to the main vessel at a controlled rate. Bromides are prepared by adding liquid bromine to a mixture of red phosphorus and the boiling alcohol at such a rate that the mixture continues to boil gently. Red phosphorus and the alcohol are heated in a flask fitted with an apparatus comprising a container A for the iodine carrying a double-surface or other reflux condenser at its upper end D and communicating via a tap B and by a tube E with a neck C for connecting to the flask. A filter plug or plate above the tap prevents clogging. Alcohol vapours condense in A and dissolve the iodine. Heating is temporarily stopped while the hot iodine solution is dropped at such a rate as to maintain gentle boiling. The reaction may be completed by distilling the contents of the flask into A and withdrawing by 3-way tap B. A may be of sufficient capacity to hold all the iodide produced when a 2-way tap suffices. Bromide can be prepared in the same apparatus, the tube E preferably being surrounded with a water condenser, or a flask fitted with dropping funnel, reflux condenser and stirrer can be used. The product is distilled, preferably with addition of water towards the end. For iodides and bromides which decompose, the product is decolourized if necessary with NaHSO3, filtered from phosphorus, advantageously after extraction with a solvent such as ether, washed, dried, and distilled under reduced pressure. Phosphorus and halogen may be used in the atomic ratio of 1 : 5 although an excess of phosphorus is preferable. Examples describe the preparation of methyl, ethyl, n- and i-propyl, n- and sec.-butyl, n-amyl, hexyl, heptyl, octyl, cyclohexyl, and b -phenylethyl iodides, b -iodopentane, trimethylene di-iodide and dibromide, and n-propyl, n- and i-butyl, n-hexyl, octyl, dodecyl, tetradecyl, hexadecyl, b -phenylethyl, tetrahydrofurfuryl, b -ethoxyethyl bromides. In this last case, a base such as pyridine or dimethylaniline may be added to the phosphorus, alcohol mixture. |
| isCitedBy | http://rdf.ncbi.nlm.nih.gov/pubchem/patent/WO-0222530-A3 http://rdf.ncbi.nlm.nih.gov/pubchem/patent/WO-0222530-A2 http://rdf.ncbi.nlm.nih.gov/pubchem/patent/US-2868850-A http://rdf.ncbi.nlm.nih.gov/pubchem/patent/US-3374278-A |
| priorityDate | 1944-01-06-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
| type | http://data.epo.org/linked-data/def/patent/Publication |
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Total number of triples: 56.