Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | Ethyl chloroformate | HCID 10928 | — |
| Reactant | HCID 54281195 | HCID 54281195 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 54177758 | HCID 54177758 | — |
Reaction Steps
36 g of the 5-amino-4-chloro-2-(2-dodecanesulfonamidobenzoylamino)phenol obtained in Step (ii) above was refluxed in 100 ml of acetonitrile and to the mixture was added dropwise 6.3 g of ethyl chloroformate. After refluxing for 4 hours, the reaction mixture was cooled to deposit the crystals. The crystals were collected by filtration and dried to yield 34 g thereof. 34 g of the crystals were dissolved in a solution composed of 4 ml of formalin, 8 ml of methylamine and 20 ml of methanol and the solution was refluxed for 5 hours with stirring. After the completion of the reaction, the reaction solution was cooled and poured into water. Acetic acid was added to the mixture to deposit the crystals. The crystals were collected by filtration, recrystallized from acetonitrile and dried to obtain 8.2 g of the above described coupler, having a melting point of 183° to 187° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04430423 |
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| Source dataset | uspto-grants-1984_02 |
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| ORD ID | ord-e7228a99877c4591ad4ba62b9f45d391 |
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| Source note | uspto-grants-1984_02 |
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