Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methanol → 5-Methoxycarbonyl2-[2-hydroxy-3-(4-chloro-alpha,alpha-dimethylbenzyl)-5-tert-butyl-phenyl]-2H-benzotriazole
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | Toluene | HCID 1140 | — |
| 반응물 | HCID 22664373 | HCID 22664373 | — |
| 생성물 | 5-Methoxycarbonyl2-[2-hydroxy-3-(4-chloro-alpha,alpha-dimethylbenzyl)-5-tert-butyl-phenyl]-2H-benzotriazole | HCID 22595032 | — |
반응 단계
The compound prepared in Example 91 (6.0 g, 0.012 mol), toluene (15 g, 0.16 mol), methanol (100 g, 3.1 mol) and concentrated sulfuric acid (0.4 g, 0.004 mol) are added to a reaction flask and heated to reflux. After eight hours at reflux, the solvents are removed by distillation and the residue is dissolved in 200 g of toluene. The solution is then passed through an absorbent (silica gel) to remove residual acid. The toluene is distilled off and the residue is twice recrystallized from methanol. The title compound is obtained in a yield of 4.9 g as a light yellow powder melting at 93-104° C. whose structure is consistent with 1Hnmr and mass spectrometric analyses.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06451887B1 |
| 출처 데이터셋 | uspto-grants-2002_09 |
| ORD ID | ord-57d548e27a2a42c1844e9c6eb317d07d |
| 출처 메모 | uspto-grants-2002_09 |