참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetonitrile | HCID 6342 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Methanesulfonyl chloride | HCID 31297 | — |
| 반응물 | 5-Bromo-2-benzothiazoleethanol | HCID 21980060 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 5-Bromo-2-[2-(2-(R)-methyl-pyrrolidin-1-yl)-ethyl]-benzothiazole | HCID 21041498 | 100% |
반응 단계
A solution of 2-(5-bromo-benzothiazol-2-yl)-ethanol (1.50 g, 5.8 mmol) and triethylamine (1.33 g, 11.6 mmol) in CH2Cl2 was cooled to 0° C., and mesyl chloride was added dropwise. The mixture was warmed to room temperature and stirred for 1 hr. The solvent was removed under vacuum, and to the residue was added acetonitrile (20 mL), triethylamine (1.33 g, 11.6 mmol) 2-(R)-methylpyrrolidine hydrochloride (2.83 g, 23.2 mmol) to the mixture, and the mixture was stirred at 60° C. for 1 hr. Solvents were removed under vacuum, and the residue was dissolved in 20 mL methylene chloride and washed with 10 mL water. The aqueous layer was re-extracted with 10 mL methylene chloride. The combined methylene chloride extracts were concentrated to give a crude product yield 1.9 g (100%)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07094790B2 |
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| 출처 데이터셋 | uspto-grants-2006_08 |
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| ORD ID | ord-648115ee2be148f0b50d9bf80b823d53 |
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| 출처 메모 | uspto-grants-2006_08 |
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