참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methane | HCID 297 | — |
| 반응물 | Ethanol | HCID 702 | — |
| 반응물 | 3-Chloro-4-methylaniline | HCID 7255 | — |
| 반응물 | HCID 178428198 | HCID 178428198 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | HCID 178428206 | HCID 178428206 | — |
반응 단계
A 500 ml., 3-neck, r.b. flask fitted with stirrer, condenser, and thermometer was charged with a mixture of the compound of Example I, C. (21.7 g., 0.1 mole), 3-chloro-4-methylaniline (14.2 g., 0.1 mole) and ethanol (300 ml.). The mixture was heated at reflux, while stirring, overnight. The near solution was concentrated to dryness by rotary evaporator and the residue was collected and dried to yield 35 g. (97.5%), m.p. 352°-364°C (dec). A 10 g. sample was dissolved in methanol (200 ml.), treated with charcoal and filtered while hot. Ether (ca 750 ml.) was added until the filtrate remained turbid and was then chilled. The crystals were collected by filtration and dried to yield 3.4 g. yellow crystals, m.p. 362°-370°C (dec). After two recrystallizations a m.p. 368°-372°C (dec) was obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US03947434 |
|---|
| 출처 데이터셋 | uspto-grants-1976_03 |
|---|
| ORD ID | ord-b80aeb6711fb4a458f42da2f0091e636 |
|---|
| 출처 메모 | uspto-grants-1976_03 |
|---|