참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | HCID 11393010 | HCID 11393010 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2-amino-2-cyano-N-(1,1-dimethylethyl)-acetamide hydrochloride | HCID 22015422 | — |
반응 단계
2-Cyano-N-(1,1-dimethylethyl)-2-[(diphenylmethylene)amino]acetamide 4 (900 g. 2.818 mol), ethyl acetate (4.5 L) and aqueous HCl (1 N. 4.5 L) were placed into a 12 L three-necked flask equipped with a nitrogen inlet, a gas outlet tube, reflux condenser, thermometer, mechanical stirrer, and maintained under a positive pressure of nitrogen. The mixture was heated on an oil bath at 60° C. for 4 hours with vigorous stirring, gradually cooled to room temperature, and then slowly diluted with CH2Cl2 (4 L). (Thin layer chromatography (EtOAc/hexanes=1/4) indicated no more starting material was present.) The resulting layers were separated and the aqueous phase was extracted with CH2Cl2 (4 L). The combined organic solutions were extracted with aqueous HCl (1 N, 2×0.5 L). The aqueous extracts were combined and concentrated under reduced pressure to yield 490 g (2.557 mol) of 2-amino-2-cyano-N-(1,1-dimethylethyl)-acetamide hydrochloride 5.HCl.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07087751B2 |
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| 출처 데이터셋 | uspto-grants-2006_08 |
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| ORD ID | ord-430da2d36fa44eec9014d4707e973baa |
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| 출처 메모 | uspto-grants-2006_08 |
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