Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1-Propanol → HCID 12521033, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1-Propanol | HCID 1031 | — |
| 반응물 | Phosphorodichloridothioic acid, O-ethyl ester | HCID 73907 | — |
| 반응물 | 1-Propanol, sodium salt (1:1) | HCID 23669363 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | HCID 12521033 | HCID 12521033 | 59.1% |
반응 단계
To 30 g (167 mmole) of O-ethyl dichlorothiophosphate in 100 ml of tetrahydrofuran (THF) cooled to -70° C. was added a solution of sodium propoxide (from 7.4 g of 60% NaH (184 mmole) and 11 g (176 mmole) of 1-propanol) in 50 ml of THF. After warming to room temperature over 2 hours, the THF was removed in vacuo and the residue was partitioned between 50 ml diethyl ether, 50 ml hexanes, and 25 ml cold water. The organic layer was dried over magnesium sulfate, concentrated in vacuo, and distilled (bp 45-50° C. 1 torr) yielding 20 g of the title compound, an oil. nmr 1.0 t 3H, 1.4 t 3H, 1.8 sextet 2H, 4.4 m 4H.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06147062 |
| 출처 데이터셋 | uspto-grants-2000_11 |
| ORD ID | ord-deff895b5cbf47998e8bbee8d1ac0ed1 |
| 출처 메모 | uspto-grants-2000_11 |