참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Sulfuryl chloride | HCID 24648 | — |
| 반응물 | Methyl 4-(4-methylphenyl)-4-oxobutanoate | HCID 288215 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 54002484 | HCID 54002484 | — |
반응 단계
A stirred solution of 152.6 g (0.74 mole) of 3-(4-methylbenzoyl)propionic methyl ester in 225 mL of methylene chloride was cooled to -5° C. in methanol:ice bath. A solution of 109.9 g (66 mL, 0.81 mole) of sulfuryl chloride (97%) in 65 mL of methylene chloride was added dropwise at a rate which maintained the temperature at 0° C. The reaction mixture was allowed to warm to ambient temperature and stirred overnight. The reaction mixture was cooled to 0° C. in an ice bath and treated with 3N sodium hydroxide until just basic. The organic portion was separated, dried over magnesium sulfate and concentrated in vacuo (172.9 g). The oil was distilled at 125° C. (150 mm Hg) in 4 fractions. A sample of fraction 2 was sent for elemental analysis.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05057534 |
|---|
| 출처 데이터셋 | uspto-grants-1991_10 |
|---|
| ORD ID | ord-10f3278064f54a2e88bfce922bcbc51e |
|---|
| 출처 메모 | uspto-grants-1991_10 |
|---|