참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | Ethanamine, 2-chloro-N-methyl-, hydrochloride (1:1) | HCID 3028223 | — |
| 반응물 | HCID 178477855 | HCID 178477855 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | HCID 178484194 | HCID 178484194 | 48% |
반응 단계
A mixture of trans-1-(4-benzo[d]isothiazol-3-yl-cyclohexyl)-8-chloro-5,6-dihydro-4H-2,3,5,10b-tetraaza-benzo[e]azulene (35.0 mg, 0.0803 mmol), cesium carbonate (105 mg, 0.321 mmol) and 2-methylaminoethyl chloride hydrochloride (41.8 mg, 0.321 mmol) in acetonitrile (0.8 ml) was heated at 70° C. for 20 h. After cooling to room temperature the reaction mixture was partitioned between 1 M aqueous sodium hydroxide solution (2 ml) and ethyl acetate (5 ml). The layers were separated. The aqueous layer was extracted with three 5-ml portions of ethyl acetate. The combined organic layers were concentrated in vacuo. Preparative RP-HPLC with water (0.05% formic acid)/methanol as eluent gave title compound (19 mg, 48%) as off-white solid. MS m/e: 493 ([M+H]+)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08481528B2 |
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| 출처 데이터셋 | uspto-grants-2013_07 |
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| ORD ID | ord-248d782c7b6b466f8041fcc0b46b782c |
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| 출처 메모 | uspto-grants-2013_07 |
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