참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | methyl 4-iodo-1H-pyrrole-2-carboxylate | HCID 11673249 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | methyl 4-iodo-1-methyl-1H-pyrrole-2-carboxylate | HCID 21826247 | — |
반응 단계
780 mg (25.9 mmol) of sodium hydride (80% in oil) and 20 ml of DMF were introduced into a three-necked flask, a solution of 6.5 g (25.9 mmol) of methyl 4-iodo-2-pyrrolecarboxylate in 50 ml of DMF was added dropwise and the mixture was stirred until gaseous emission ceased. 2.1 ml (33.6 mmol) of iodomethane were then added and the mixture was stirred at room temperature for two hours. The reaction medium was poured into water, extracted with ethyl ether, the organic phase decanted, dried over magnesium sulfate and evaporated. The residue obtained was purified by chromatography on a silica column eluted with a mixture of dichloromethane and hexane (40/60). 4.5 g (65%) of methyl N-methyl-4-iodo-2-pyrrolecarboxylate of melting point 64°-65° C. were recovered.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05723499 |
|---|
| 출처 데이터셋 | uspto-grants-1998_03 |
|---|
| ORD ID | ord-8254c501c8dc491b8f88eae119f49eae |
|---|
| 출처 메모 | uspto-grants-1998_03 |
|---|