Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Thionyl Chloride | HCID 24386 | — |
| Reactant | HCID 20291877 | HCID 20291877 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 20291879 | HCID 20291879 | 77.9% |
Reaction Steps
15.0 g (0.05 mol) of the 6-(3-azidophthalimidyl)-caproic acid obtained according to Example 8 are dissolved in 327 g (2.75 mols) of thionyl chloride, and the solution is warmed to 80° C., the operations being carried out under yellow light. At 80° C., 0.5 ml of N,N-dimethylformamide is added to the clear solution obtained. The reaction mixture is stirred for 15 minutes at 80° C. and is then cooled to room temperature. This produces a beige-coloured suspension, which is filtered with suction, under N2. The crude product is recrystallised from 250 ml of dry ligroin. 12.5 g (75.4% of theory) of 6-(3-azidophthalimidyl)-caproyl chloride are obtained; melting point 68°-69° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04250096 |
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| Source dataset | uspto-grants-1981_02 |
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| ORD ID | ord-3a8bacd80418467284e0f37409c20db3 |
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| Source note | uspto-grants-1981_02 |
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