참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Urea | HCID 1176 | — |
| 반응물 | 4-Chloro-5-nitrophthalimide | HCID 2801129 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 5-Amino-6-nitro-1H-isoindole-1,3(2H)-dione | HCID 15144568 | — |
반응 단계
The following procedure is our modification: A mixture of 5-chloro-6-nitroisoindoline-1,3-dione (28.0 g, 0.123 mol) and urea (73.8 g, 1.23 mol) was stirred at 150° C. for 6 h. Then the temperature was reduced to 90° C., water (400 mL) was added, the mixture was stirred overnight at RT. Precipitate was collected by filtration, water (300 mL) was added and stirred for 4 h at 95° C. The solid was collected by filtration and dried under vacuum. Yellow solid, 19.6 g (94.7 mmol, 77%). LCMS [M−H]− 205.9. 1H NMR (300 MHz, DMSO): δ 11.46 (s, 1H), 8.35 (s, 2H), 8.37 (s, 1H), 7.40 (s, 1H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08063225B2 |
|---|
| 출처 데이터셋 | uspto-grants-2011_11 |
|---|
| ORD ID | ord-df5ffcf802864f00a5414048bd10cd11 |
|---|
| 출처 메모 | uspto-grants-2011_11 |
|---|