참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 3-(Dimethylamino)-2-propenal | HCID 79125 | — |
| 반응물 | Borate(1-), tetrafluoro-, hydrogen, compd. with pyridine (1:1:1) | HCID 11019233 | — |
| 반응물 | AcOH AcOAc | HCID 21895370 | — |
| 생성물 | HCID 178500406 | HCID 178500406 | 65% |
반응 단계
Pyridiniumtetrafluoroborate (283.7 g, 1.70 mol) was added to a solution of methyl-(2E)-3-(3-dimethylamino)prop-2-enoate in 442.5 ml acetic anhydride/acetic acid (2:1). The resulting suspension was cooled to 0° C. and 3-dimethylaminoacroleine (169.9 ml, 1.70 mol) was added slowly over the course of 3 hrs. under vigorous stirring and cooling with an ice bath, a yellow-brown precipitate formed. After further stirring for 2 hrs. at room temperature the reaction mixture was filtered. The remaining solid was washed with diethylether several times and dried under reduced pressure. Re crystallization from i-propanol/ethanol (2:1) gave 326.7 g (65%) of the pentamethinium salt as yellow crystals.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08580949B2 |
|---|
| 출처 데이터셋 | uspto-grants-2013_11 |
|---|
| ORD ID | ord-a5d6e144d551412a9f4896dbda643d07 |
|---|
| 출처 메모 | uspto-grants-2013_11 |
|---|
