Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Iodine → 3-Iodo-1-methyl-2-pyridin-4-yl-1H-pyrrolo[3,2-b]pyridine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Iodine | HCID 807 | — |
| 반응물 | Sodium Thiosulfate | HCID 24477 | — |
| 반응물 | Dimethyl-(2-pyridin-4-ylethynyl-pyridin-3-yl)-amine | HCID 68429284 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 3-Iodo-1-methyl-2-pyridin-4-yl-1H-pyrrolo[3,2-b]pyridine | HCID 68430585 | 40.7% |
반응 단계
1 g (4.4 mmoles) of Dimethyl-(2-pyridin-4-ylethynyl-pyridin-3-yl)-amine are dissolved in 60 mL of dichloromethane under argon atmosphere. A solution of 2.27 g of iodine (8.9 mmoles) in 35 mL of dichloromethane is added dropwise in the reaction mixture at 0° C. The reaction mixture is allowed to reach room temperature and further stirred for 4 hours. The reaction mixture is then poured into a solution sodium thiosulfate and extracted with dichloromethane. The organic phase is washed with water and dried over magnesium sulfate. The solid residue after concentration is purified by chromatography on silica gel (ethylacetate) to give 600 mg of 3-Iodo-1-methyl-2-pyridin-4-yl-1H-pyrrolo[3,2-b]pyridine as brown solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08084395B2 |
| 출처 데이터셋 | uspto-grants-2011_12 |
| ORD ID | ord-0f92119da96a421f9e3b88b7f28a0351 |
| 출처 메모 | uspto-grants-2011_12 |