Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → 1-[2-(4-Bromo-2-chloromethylphenoxy)ethyl]pyrrolidine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Thionyl Chloride | HCID 24386 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | 1-[2-(2-Hydroxymethyl-4-bromophenoxy)ethyl]pyrrolidine | HCID 21182863 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 1-[2-(4-Bromo-2-chloromethylphenoxy)ethyl]pyrrolidine | HCID 69059822 | — |
반응 단계
0.16 mL (2.20 mmol) of thionyl chloride was added at −10° C. to a solution of 0.60 g (2.00 mmol) of [5-bromo-2-(2-pyrrolidin-1-ylethoxy)phenyl]methanol and 0.42 mL (3.00 mmol) of triethylamine in 30 mL of THF and the mixture was stirred for 16 hours at RT. Ice and dilute aqueous sodium bicarbonate solution was added to the reaction mixture and the phases were separated. The aqueous phase was exhaustively extracted with DCM, and the combined organic phases were washed with water, dried over magnesium sulfate, and evaporated down in vacuo. Yield: 0.39 g (62% of theoretical); C13H17BrClNO (M=318.637); calc.: molpeak (M+H)+: 318/320/322 (BrCl); found: molpeak (M+H)+: 318/320/322 (BrCl); HPLC-MS: 5.84 minutes (method A).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07592358B2 |
| 출처 데이터셋 | uspto-grants-2009_09 |
| ORD ID | ord-59de8ca491d041b88695725a4313be7d |
| 출처 메모 | uspto-grants-2009_09 |