Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ammonia → Malonyldiamide, N,N'-bis(trimethylsilyl)-
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ammonia | HCID 222 | — |
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | Malonamide | HCID 7911 | — |
| 반응물 | Hexamethyldisilazane | HCID 13838 | — |
| 촉매 | Saccharin | HCID 5143 | — |
| 용매 | Pyridine | HCID 1049 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | Malonyldiamide, N,N'-bis(trimethylsilyl)- | HCID 554458 | 99,004.203% |
반응 단계
7.5 ml (36 mmoles) of hexamethyldisilazane were added to a refluxing mixture of 3.06 g (0.03 mmole) of malonamide, 18.3 mg (0.1 mmole) of saccharin, 50 ml of ethyl acetate and 5 ml of pyridine and by titrating with 1 N sulfuric acid the ammonia evolved, it was found that 30 mmoles were expelled after refluxing for one hour. Volatile material was vacuum evaporated and the residue, which crystallized upon standing, was dried in vacuo to obtain 7.32 g (99%) of N,N'-bis-(trimethylsilyl)-malonamide melting at 72°-76° C. NMR Spectrum (CDCl3): Δ0.24 (s, 18H); 3.20 (s, 2H); 6.5 (broad, 2H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04400509 |
| 출처 데이터셋 | uspto-grants-1983_08 |
| ORD ID | ord-26864b483c4f4499ba9816be3ef8ef45 |
| 출처 메모 | uspto-grants-1983_08 |