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Hydrochloric Acid → {3-[(6-Chloro-benzooxazol-2-ylamino)-methyl]-pyrrolidin-1-yl}-(2,6-dimethoxy-phenyl)-methanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2,6-Dimethoxybenzoyl chloride | HCID 74810 | — |
| 反応物 | (6-Chloro-benzooxazol-2-yl)-pyrrolidin-3-ylmethyl-amine | HCID 59178006 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | {3-[(6-Chloro-benzooxazol-2-ylamino)-methyl]-pyrrolidin-1-yl}-(2,6-dimethoxy-phenyl)-methanone | HCID 44610702 | 22.3% |
反応手順
A mixture of 20 mg (0.07 mmol) (6-chloro-benzooxazol-2-yl)-pyrrolidin-3-ylmethyl-amine; hydrochloride, 15 mg (0.77 mmol) 2,6-dimethoxybenzoyl chloride and 10 mg (0.1 mmol) NEt3 in 2 mL DCM was shaken at room temperature over night. After evaporation the residue was subjected to purification by preparative HPLC on reversed phase eluting with a gradient formed from acetonitrile, water and formic acid. The product containing fractions were evaporated to yield 6.5 mg (22%) of the title compound. MS (m/e): 416.2 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08748430B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-81b5459bc2b04aee9fa5626f35421bb0 |
| 出典メモ | uspto-grants-2014_06 |