Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Tetrahydrofuran → (3R,5S)-7-Chloro-5-(2-chlorophenyl)-3-(2-hydroxyethyl)-1-neopentyl-1,2,3,5-tetrahydro-4,1-benzoxazepine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | trans-7-Chloro-5-(2-chlorophenyl)-1-neopentyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-acetic acid | HCID 10048630 | — |
| 반응물 | Aluminium lithium hydride | HCID 21226445 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | (3R,5S)-7-Chloro-5-(2-chlorophenyl)-3-(2-hydroxyethyl)-1-neopentyl-1,2,3,5-tetrahydro-4,1-benzoxazepine | HCID 53790172 | 88.2% |
반응 단계
To tetrahydrofuran (20 ml) were added (3R,5S)-7-Chloro-5-(2-chlorophenyl)-1-neopentyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-acetic acid (2 g) and aluminum lithium hydride (0.4 g). The mixture was heated for 6 hours under reflux, to which was added water. Insolubles were then filtered off. The filtrate was concentrated, which was purified by means of a silica gel column chromatography (hexane:acetic acid ethyl ester=2:1 v/v as an eluent) to give 1.65 g of non-crystalline solid matter.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05698691 |
| 출처 데이터셋 | uspto-grants-1997_12 |
| ORD ID | ord-47d32c717fcd4e328951d12ee3b810c4 |
| 출처 메모 | uspto-grants-1997_12 |