Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Cyclopentanone → Methyl 4-(N-cyclopentylamino)-3-iodobenzoate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Cyclopentanone | HCID 8452 | — |
| 반응물 | Sodium Sulfate | HCID 24436 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | Methyl 4-amino-3-iodobenzoate | HCID 4104649 | — |
| 반응물 | Sodium triacetoxyborohydride | HCID 5049666 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 생성물 | Methyl 4-(N-cyclopentylamino)-3-iodobenzoate | HCID 21974264 | — |
반응 단계
A mixture of methyl 4-amino-3-iodobenzoate from above (27.69 g, 100 mmol), cyclopentanone (52.8 mL, 600 mmol), and anhydrous sodium sulfate (1000 g, 142 mmol) in 500 mL of glacial acetic acid was stirred for two hours. Solid sodium triacetoxyborohydride (76.92, 345 mmol) was added in portions and stirred for 16 hrs at room temperature. The mixture was poured on to cool 900 mL of saturated aqueous sodium bicarbonate solution carefully and extracted with 150 mL (3×) of ethyl acetate. The ethyl acetate fraction was dried and evaporated. Purification with silica gel and 0.5% ethyl acetate in hexane gave 24 g (70%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07098231B2 |
| 출처 데이터셋 | uspto-grants-2006_08 |
| ORD ID | ord-2a913d18f5f04d3f8b60c7d5ab1a93c6 |
| 출처 메모 | uspto-grants-2006_08 |