Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| Reactant | HCID 57000686 | HCID 57000686 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 18650837 | HCID 18650837 | 47.4% |
Reaction Steps
0.50 g of the (R,S) -4-[4'-(3"-hydroxy-1"-methylbutoxy)phenyl]benzonitrile obtained in the above Example 1 was mixed with 0.12 g of acetic anhydride, 0.51 g of triphenylphosphine and 5 ml of ethyl ether. To the obtained mixture, was added dropwise 0.34 g of diethyl azodicarboxylate under stirring. The obtained mixture was stirred at room temperature for three hours. The triphenylphosphine oxide thus precipitated was filtered and desolvated to thereby give a crude product which was purified by silica gel column chromatography with the use of a mixture of ethyl acetate and n-hexane (1:3) as a developing solvent. Thus 0.18 g of the title compound as obtained. The obtained product showed the following characteristic absorptions in infrared spectroscopy, which proved that it was the aimed compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05401436 |
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| Source dataset | uspto-grants-1995_03 |
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| ORD ID | ord-9aba039714434def90c1ea08df181455 |
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| Source note | uspto-grants-1995_03 |
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