참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ammonia | HCID 222 | — |
| 반응물 | 5,8,14-Triazatetracyclo[10.3.1.02, 11.04,9]hexadeca-2(11),3,5,7,9-pentaene tosylate salt | HCID 86637774 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 5,8,14-Triazatetracyclo[10.3.1.02,11.04,9]hexadeca-2,4,6,8,10-pentaene | HCID 170361 | — |
반응 단계
In a 250 ml 4 neck round bottom flask equipped with mechanical stirrer, Thermo pocket were charged DM water (30 ml) and 5,8,14-Triazatetracyclo[10.3.1.02,11.04,9]hexadeca-2(11),3,5,7,9-pentaene Tosylate salt (10 g, having a total purity of 99.42% obtained in example 4). The above suspension was stirred for 30 minutes at 25-30° C. To this was added 25% aqueous ammonia solution (5 ml) to adjust the pH to 9.0-10 at 25-30° C., and MDC (30 ml) was added to this solution. The resulting mixture was stirred for 30 minutes at 20-25° C. The organic layer was separated, and the aqueous layer was extracted with MDC (4×30 ml). The combined organic layer was washed with DM water (30 ml). The organic layer was treated with activated carbon (1.0 g), and stirred for 30 minutes at 25-30° C. The resulting solution filtered through celite. Concentration afforded a solid product, i.e. 5,8,14-Triazatetracyclo[10.3.1.02,11.04,9]hexadeca-2(11),3,5,7,9-pentaene. (Yield-5 g (95.06% (relative to VRN-Tosylate)), HPLC purity-99.43%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08039620B2 |
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| 출처 데이터셋 | uspto-grants-2011_10 |
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| ORD ID | ord-cddf5066e0844a01a2198b36c685bcad |
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| 출처 메모 | uspto-grants-2011_10 |
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