Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Carbon Tetrachloride | HCID 5943 | — |
| Reactant | Hexamethylphosphorous triamide | HCID 15355 | — |
| Reactant | HCID 54422830 | HCID 54422830 | — |
| Solvent | Pentane | HCID 8003 | — |
| Product | HCID 57218863 | HCID 57218863 | 94.7% |
Reaction Steps
Tri(dimethylamino)phosphine (163.2 mmol) was added with stirring at 0° C. to a solution of (1R,cis)-2-(2,2-dimethoxyethyl)-3,3-dimethylcyclopropanecarbaldehyde (65.5 mmol) and carbon tetrachloride (163.2 mmol) in n-pentane (350 ml) kept under nitrogen in a 1-l flask. After 15 minutes stirring, the mixture was warmed up to 14° C. and kept at this temperature for 15 minutes. Then, water (75 ml) was added at 14° C. and--after removal of the aqueous phase--the organic phase was washed with two 35-ml portions of water. The washed organic phase was dried over anhydrous magnesium sulphate and the solvent was evaporated from the dried solution to give a residue (15.7 g) containing 32.1 mmol of 2-[2-(2,2-dichlorovinyl)-3,3-dimethylcyclopropyl]ethanal dimethyl acetal (100% (1R,cis), purity 51.7%, yield 49%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04234512 |
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| Source dataset | uspto-grants-1980_11 |
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| ORD ID | ord-c724c0d80e6047478c23df3f9a5e98d7 |
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| Source note | uspto-grants-1980_11 |
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