Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | 2-(3-Chlorophenoxymethyl)oxirane | HCID 9899028 | — |
| Reactant | HCID 20060610 | HCID 20060610 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 131716048 | HCID 131716048 | 55% |
Reaction Steps
A mixture of 2.77 parts of [(3-chlorophenoxy)methyl]oxirane, 4.92 parts of N-(3-methyl-2(3H)-benzothiazolylidene)-4-piperidinamine monohydrobromide, 2.12 parts of sodium carbonate, 60 parts of methanol and 68 parts of methylbenzene was stirred and refluxed overnight. The reaction mixture was cooled and the solvent was evaporated. The residue was purified by filtration over silica gel using a mixture of trichloromethane and methanol (99:1 by volume), as eluent. The pure fractions were collected and the eluent was evaporated. The residue was converted into the (Z)-2-butenedioate salt in 2-propanol and methanol. The salt was filtered off and dried, yielding 5.5 parts (55%) of α-[(3-chlorophenoxy)methyl]-4-[(3-methyl-2(3H)-benzothiazolyliden)amino]-1-piperidineethanol (Z)-2-butenedioate(1:2); mp. 157.6° C. (428).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04861785 |
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| Source dataset | uspto-grants-1989_08 |
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| ORD ID | ord-25375767ed0b433e9f36ef23a976339d |
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| Source note | uspto-grants-1989_08 |
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