참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Acetonitrile | HCID 6342 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Methyl 4-(1-methylethoxy)benzoate | HCID 3015807 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 4-(1-Methylethoxy)-beta-oxobenzenepropanenitrile | HCID 20387514 | — |
반응 단계
To a solution of 4-Isopropoxy-benzoic acid methyl ester (2.2 g, 11.2 mmol, 1.0 eq) in dry toluene (15 mL) under N2, NaH (50-60% dispersion in mineral oil, 1.1 g, 22.4 mmol, 2.0 eq) was added. The mixture was heated at 80° C. and then dry CH3CN was added dropwise (2.8 mL, 56.0 mmol, 5.0 eq). The reaction was heated for 18 hours, then was allowed to cool down to room temperature and acidified with HCl 2N. The organic phase was recovered and 2.0 g of crude were obtained and it was used for cyclization without further purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08163729B2 |
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| 출처 데이터셋 | uspto-grants-2012_04 |
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| ORD ID | ord-009cc470c01b4f7bba83b356848fb8bf |
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| 출처 메모 | uspto-grants-2012_04 |
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