Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Methacryloyl chloride | HCID 13528 | — |
| Reactant | HCID 10680815 | HCID 10680815 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Product | HCID 19010701 | HCID 19010701 | — |
Reaction Steps
1000 ml of dried methylene chloride are placed in a 4 l sulfonating vessel at 0° C. together with 334 g of methacrylic acid chloride. A mixture of 500 ml of dried methylene chloride, 323 of dried triethylamine and 454 of N-benzyl-N(β-hydroxyethyl)aniline, (the compound of formula 1a) are added drop by drop to this mixture at 0°-10° C. The reaction mixture is allowed to rise to room temperature slowly and is controlled on a thin layer chromatograph (silica gel) solvent: toluene/acetic acid ester 2:1. After the end of the reaction (after standing overnight), the reaction mixture is filtered and washed three times with one liter of a 10% aqueous NaOH solution and finally four times each time with 1 l of water. The organic phase is then dried over sodium sulphate and the solvent is removed in a rotary evaporator. 482 g of the product of formula 1d ##STR15## results.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05334710 |
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| Source dataset | uspto-grants-1994_08 |
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| ORD ID | ord-96337e7de061488c94b6a1916c296798 |
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| Source note | uspto-grants-1994_08 |
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