참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | 1-Phenoxy-2-propanone | HCID 69313 | — |
| 반응물 | HCID 178418573 | HCID 178418573 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | 2-Methyl-1-phenoxy-2-propanol | HCID 10374790 | 91.4% |
반응 단계
To a stirred solution of 24.2 g (0.16 mole) of phenoxy-2-propanone (Eastman) in 150 mL of dry ethyl ether was added 56 ml (0.17 mole) of methylmagnesium bromide (3.0M solution in ethyl ether, Aldrich) and the reaction mixture was stirred at ambient temperature under a nitrogen atmosphere for 4 hr. The reaction mixture was treated with 100 ml of saturated ammonium chloride solution and vigorously stirred for 1 hr. The layers were separated and the organic layer was washed twice with 200 ml portions of water, dried (magnesium sulfate) and the solvent evaporated under reduced pressure to yield 24.3 g (91%) of a vicous oil. A 2.3 g sample of the oil was purified by high pressure liquid chromatography (Waters Associates Prep LC/System 500 A, PrePAK 500/silica, ethyl acetate-hexanes, 1:20, flow rate 150 ml/min). The desired fractions were combined and the solvents evaporated under reduced pressure to yield 2.1 g (91% recovery) of the title compound as a colorless liquid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05273993 |
|---|
| 출처 데이터셋 | uspto-grants-1993_12 |
|---|
| ORD ID | ord-d24d54f071a64d79897b34f899bc6728 |
|---|
| 출처 메모 | uspto-grants-1993_12 |
|---|