Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | HCID 21200304 | HCID 21200304 | — |
| Product | HCID 15410533 | HCID 15410533 | — |
Reaction Steps
20 g of the derivative prepared according to (a) in 80 ml of acetic acid are introduced into a round-bottomed flask. 6.75 ml of 80% sulphuric acid are then added dropwise and the reaction mixture is heated to 80° C. and then under reflux for 1 hour and 30 minutes. The reaction mixture is then left to return to room temperature and 240 ml of iced water are added to it. After stirring at 10° C. for 30 minutes, the precipitate is separated off by filtration. The precipitate is taken up into 130 ml of acetic acid which is then distilled off in order to obtain a residue which crystallises providing 17 g of the expected product (Formula (I), X=CH2, Ar=3,4-dichlorophenyl); M. Pt.=203° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06008360 |
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| Source dataset | uspto-grants-1999_12 |
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| ORD ID | ord-c4adced8fa1d42cc9270d74eb35d50e4 |
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| Source note | uspto-grants-1999_12 |
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