Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → 2-Ethyl-2-((2-Hydroxymethylphenyl)thiomethyl)hexenal
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 2-Mercaptobenzenemethanol | HCID 138278 | — |
| 반응물 | Mercaptobenzyl alcohol | HCID 5251295 | — |
| 반응물 | 2-Ethyl-2-(mesyloxymethyl)hexanal | HCID 11572217 | — |
| 용매 | Diglyme | HCID 8150 | — |
| 용매 | Triethylamine | HCID 8471 | — |
| 생성물 | 2-Ethyl-2-((2-Hydroxymethylphenyl)thiomethyl)hexenal | HCID 54430931 | 107.8% |
반응 단계
A mixture of 5.0 g (0.036 mole) of 2-mercaptobenzyl alcohol, 6.4 g (0.032 mole) of 1, 3.6 g (0.036 mole) of triethylamine and 25 mL of 2-methoxyethyl ether was held at reflux for 7 h. Additional 1.1 g of mercaptobenzyl alcohol and 0.72 g of triethylamine was added to the reaction mixture and the mixture was held at reflux for additional 16 h. The reaction mixture was cooled and poured into 6N HCl and extracted with methylene chloride. The methylene chloride extract was washed twice with 10% NaOH, dried over MgSO4 and concentrated in vacuo to give 9.6 g of residue. Purification by HPLC (20% EtOAc-hexane) gave 3.7 g (41%) of 16 as an oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06642268B2 |
| 출처 데이터셋 | uspto-grants-2003_11 |
| ORD ID | ord-f7dd7cd9bbc04888b4817b8ee5124c3b |
| 출처 메모 | uspto-grants-2003_11 |