참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Dexmethylphenidate | HCID 154101 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Isopropanol | HCID 3776 | — |
| 생성물 | Focalin | HCID 154100 | 86% |
반응 단계
The organic layer was dewatered by azeotropic distillation under vacuum and was concentrated in vacuum to give D-threo-methylphenidate free base as an oil, which was used directly in hydrochloride salt formation. The solution of D-threo-methylphenidate free base in isopropanol (0.29 Kg) was charged to a jacketed vessel, cooled to 5-10° C. and treated with a solution of 37% HCl (78 g) in a mixture of isopropanol (40 g) and methanol (63 g) at less than 20° C. The formed slurry was cooled to 0 to 5° C., aged for 2 hours and filtered. The wet cake was washed with isopropanol (0.32 Kg total) in two portions and dried under vacuum at 45° C. for 16 hours to give Dexmethylphenidate hydrochloride (0.175 Kg, 0.649 mol, 86% yield) as a off-white solid; mp 206.4° C., ee 99.7%, α25D +83° (c 1 wt %, MeOH).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07897777B2 |
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| 출처 데이터셋 | uspto-grants-2011_03 |
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| ORD ID | ord-ed253010351a4d048e21b0b089654b1e |
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| 출처 메모 | uspto-grants-2011_03 |
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