Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ammonium Chloride → 6-Methyl-1,3-dioxaindan-5-amine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | 5-Methyl-6-nitro-1,3-benzodioxole | HCID 4550461 | — |
| 촉매 | Iron | HCID 23925 | — |
| 용매 | Methanol--water (1/1) | HCID 22242641 | — |
| 생성물 | 6-Methyl-1,3-dioxaindan-5-amine | HCID 12445340 | 94.5% |
반응 단계
A mixture of 5-methyl-6-nitro-benzo(1,3)dioxole (50 mg, 0.28 mmol), Fe (54 mg, 3.5 eq) and ammonium chloride (51.2 mg, 3.5 eq) in a 1:1 mixture of MeOH/H2O (2.8 mL) was subjected to microwave irradiation (60W, P=100 p.s.i.) at 80° C. for four 10 min periods. The brown solution was allowed to cool to r.t. and more Fe (3.5 eq) and ammonium chloride (3.5 eq) were added. The mixture was subjected to microwave irradiation (60W, P=100 p.s.i.) at 80° C. for an additional 10 min. Fe was filtered off and the solvent evaporated. The crude product was purified on an SCX cartridge (cHex/EtOAc 9:1) to give the title compound as a brown solid (40 mg, 93%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07427630B2 |
| 출처 데이터셋 | uspto-grants-2008_09 |
| ORD ID | ord-dc47ee82b9a8400b886e1229bfe8af8c |
| 출처 메모 | uspto-grants-2008_09 |