Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methanesulfonic Acid → 5-(N,N-Diethylaminomethyl)-3-(2,5-dimethoxybenzylamino)-2-diphenylmethyl-1-azabicyclo[2.2.2]octane
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methanesulfonic Acid | HCID 6395 | — |
| 반응물 | Sodium Sulfate | HCID 24436 | — |
| 반응물 | N,N-Diethyl-5-(2,5-dimethoxy benzylamino)-6-diphenylmethyl-1-azabicyclo[2.2.2]octane-3-carboxamide | HCID 10165826 | — |
| 용매 | Acetone | HCID 180 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 5-(N,N-Diethylaminomethyl)-3-(2,5-dimethoxybenzylamino)-2-diphenylmethyl-1-azabicyclo[2.2.2]octane | HCID 70115721 | 57% |
반응 단계
A solution of 19 (300 mg, 0.55 mmole) in dry THF (2 ml) was added to a suspension of LiAIH4 (105 mg, 2.75 mmole) in 5 ml of dry THF at 5° C. and stirred at room temperature for 1 hour. Na2SO4 /10H2O (2 g) was added to the reaction mixture and stirred for 15 hours at room temperature. The suspension was filtrated, and the solids were washed with dry THF. The filtrate was concentrated under reduced pressure. The resulting oil was dissolved in 2 ml of acetone, and CH3SO3H (159 mg, 1.65 mmole) was added to the solution of the crude oil in acetone (2 ml). The resulting precipitate was collected by filtration and dried in vacuo to give 20 (254 mg, 0.31 mmole, 57%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05852038 |
| 출처 데이터셋 | uspto-grants-1998_12 |
| ORD ID | ord-fdc3a328f762429494463eeedb04a933 |
| 출처 메모 | uspto-grants-1998_12 |