Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Thiophenol → 1-Dimethylamino-3-phenyl-3-phenylthio-2-propene
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Thiophenol | HCID 7969 | — |
| 반응물 | 3-(Dimethylamino)-1-phenyl-2-propen-1-one | HCID 353460 | — |
| 반응물 | Sodium cyanoborohydride | HCID 5003444 | — |
| 용매 | Phosphorus oxychloride | HCID 24813 | — |
| 생성물 | 1-Dimethylamino-3-phenyl-3-phenylthio-2-propene | HCID 54193170 | — |
반응 단계
By using a method similar to that described in Example 35, but starting from 3-dimethylaminoacrylophenone (80 g), phosphorus oxychloride (40 cc), thiophenol (50.3 cc) and sodium cyanoborohydride (16 g), and crystallising the (Z)-isomer, a yellow solid is isolated after evaporation of the mother liquors under reduced pressure (2.7 kPa) at 30° C. followed by crystallisation of the residue obtained from a mixture of acetone and ethyl ether (25/75 by volume); the solid is recrystallised from methyl ethyl ketone (230 cc). 1-Dimethylamino-3-phenyl-3-phenylthio-2-propene (E) hydrochloride (14.3 g) is thus obtained in the form of a white solid melting at 146°-147° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04755599 |
| 출처 데이터셋 | uspto-grants-1988_07 |
| ORD ID | ord-5f17f24339934a9d89f744c2037afce9 |
| 출처 메모 | uspto-grants-1988_07 |