참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 4-Amino-3,5-dichloropyridine | HCID 89888 | — |
| 반응물 | Potassium | HCID 5462222 | — |
| 반응물 | 3-(Cyclopropylmethoxy)-4-(difluoromethoxy)benzoyl chloride | HCID 12047330 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | Roflumilast | HCID 449193 | — |
반응 단계
The potassium salt suspension of the anion of 4-amino-3,5-dichloropyridine in DMF (2-2.5 equivalents) is introduced into a reaction vessel. A solution of 3-cyclopropylmethoxy-4-difluoromethoxybenzoyl chloride (1 equivalent) in DMF is slowly added to this suspension while stirring vigorously at a temperature of 15 to 40° C., preferably 20 to 30° C. After the reaction is complete, water is slowly added while stirring at 15-25° C., and the pH is adjusted to 2-3 with hydrochloric acid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08536206B2 |
|---|
| 출처 데이터셋 | uspto-grants-2013_09 |
|---|
| ORD ID | ord-cd988c3896aa452ba5e90738334d9fe9 |
|---|
| 출처 메모 | uspto-grants-2013_09 |
|---|
