Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | 2,2'-(Cyclopropane-1,1-diyl)diacetic acid | HCID 12530991 | — |
| Solvent | Mesitylene | HCID 7947 | — |
| Product | 144728-22-3 | HCID 54153109 | — |
Reaction Steps
350 g crude (1-carboxymethyl-cyclopropyl)-acetic acid (2.2 mole, 92% purity, from step 1) are suspended in a mixture of 350 ml of mesitylene and 678 g of acetic anhydride (6.6 mole, 3 eq) and heated to 100° C. Upon reaching that temperature, the pressure is reduced to approximately 200 mbar and 45% of the solvent mixture are distilled off (distillation takes approx. 1 h). Then the mixture is slowly cooled to 0-5° C. and the precipitate is collected by filtration. The filter cake is washed with 87 ml of cold mesitylene and then dried in vaccuo at 40° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09212120B2 |
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| Source dataset | uspto-grants-2015_12 |
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| ORD ID | ord-8bb45a0a82fb4c56a3dd30f81ced4e0b |
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| Source note | uspto-grants-2015_12 |
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