참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 2-Methylfuran-3-carbonyl chloride | HCID 2759850 | — |
| 반응물 | 4-Chloro-3-(3-methyl-2-butenyloxy)benzenamine | HCID 12985691 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 86751707 | HCID 86751707 | — |
반응 단계
A first solution of 2-methyl-3-furancarboxylic chloride (13.57 g) in methylene chloride (94 mL) was stirred in an ice/salt bath. A second solution of 4-chloro-3-(3-methyl-2-butenyloxy)benzenamine (19.8 g), triethylamine (14 mL) in methylene chloride (94 mL) was added to the first solution at such a rate that the temperature was maintained at -5° C. to 0° C. When the addition was complete, the resultant reaction mixture was stirred to ambient temperature and left stirring for 15 hours. Water was added to the reaction mixture and then the organic layer separated and washed successively with water, dilute hydrochloric acid, water, aqueous sodium bicarbonate, and water. After drying (MgSO4), the solvent was removed from the washed organic layer and the residue was recrystallised from isopropyl alcohol to give N-[4-chloro-3-(3-methyl-2-butenyloxy)phenyl-2-methyl-3-furancarboxamide, a white solid, 17 g. A second crop of beige crystals, 7.6 g, was also obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05696151 |
|---|
| 출처 데이터셋 | uspto-grants-1997_12 |
|---|
| ORD ID | ord-48006369236940739f0dc822040ec83b |
|---|
| 출처 메모 | uspto-grants-1997_12 |
|---|