참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 2-Chloroethanol | HCID 34 | — |
| 반응물 | Acetone | HCID 180 | — |
| 반응물 | Acetone Cyanohydrin | HCID 6406 | — |
| 촉매 | Zincchloride | HCID 3007855 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 2-(2-Chloroethoxy)-2-methylpropanenitrile | HCID 21069786 | 46.6% |
반응 단계
Additional procedure. ZnCl2 (352.3 g 2.59 moles) was added to a 2 L round bottom flask equipped with a mechanical stirrer, nitrogen inlet-outlet, temperature probe, and condenser. Acetone cyanohydrin (110.0 g 1.29 moles) was slowly added to the stirred solid over 30 minutes keeping the temperature below 32° C. with external cooling. To the slurry, 2-chloroethanol (124.9 g 1.55 moles) was slowly added over 20 minutes keeping the temperature below 32° C. with external cooling. Acetone (3.75 g, 64.6 mmoles) was added and the mixture was heated to 60° C. After stirring for 4 h at 60° C., the reaction mixture was cooled to 30-35° C., diluted with water (1.10 L) and extracted with CH2Cl2 (1×440 mL and 1×220 mL). The combined CH2Cl2 extracts were washed with 0.5M sodium bicarbonate (330 mL), followed by water (3×330 mL). The dichloromethane solution was concentrated under vacuum to afford crude product (109 g). The crude product was purified by vacuum distillation (10 mm Hg) using a Vigreux column. The fraction boiling at 60-80° C. was collected to afford 2-(2-chloroethoxy)-2-methylpropanenitrile as colorless oil (88.7 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07893055B2 |
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| 출처 데이터셋 | uspto-grants-2011_02 |
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| ORD ID | ord-9174c53b09f6487caa82e6b0cfa0c23b |
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| 출처 메모 | uspto-grants-2011_02 |
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