참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 2-Amino-m-cresol | HCID 3014138 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 4-Methyl-3H-benzooxazol-2-one | HCID 12709336 | — |
반응 단계
25.0 g (200 mmol) 2-amino-m-cresol and 70.4 mL (400 mmol) DIPEA were placed in 1.0 L DCM and cooled to 0° C. To this a solution of 38.0 g (227 mmol) CDI was added dropwise over 30 min. The mixture was stirred for 30 min at 0° C., then stirred overnight at RT. After evaporation of the reaction mixture i. vac. down to half the volume, the aqueous phase was washed with water (2×250 mL), 1M aqueous potassium hydrogen sulphate solution (1×250 mL) and again water (1×250 mL). The organic phase was evaporated down i. vac. The crude product left as a solid was triturated with a mixture of diethyl ether and PE, the precipitated solid was suction filtered, washed with PE and dried i. vac.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08629137B2 |
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| 출처 데이터셋 | uspto-grants-2014_01 |
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| ORD ID | ord-5974944588dd404589cdfbbbbdd14c62 |
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| 출처 메모 | uspto-grants-2014_01 |
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