참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ammonia | HCID 222 | — |
| 반응물 | Ethanol | HCID 702 | — |
| 반응물 | 2,2-dimethyl-2H-1-benzopyran-6-carbonitrile | HCID 2779074 | — |
| 촉매 | Nickel | HCID 935 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | (2,2-dimethyl-2H-chromen-6-yl)methanamine | HCID 55255597 | 97.9% |
반응 단계
Add 2,2-dimethyl-2H-chromene-6-carbonitrile (1.5 g, 8.1 mmol) and ethanol wet Raney® activated nickel (0.4 g) to a Parr pressure vessel. Immediately add 7N ammonia in methanol (170 mL) and seal the vessel. Purge the reaction vessel with nitrogen, pressurize the reaction mixture with hydrogen (3400 KPa), seal the vessel, agitate the reaction and heat to 60° C. for 20 h. Turn off the heat and allow the reaction mixture to cool to ambient temperature. Vent the excess hydrogen from the vessel and purge the vessel with nitrogen. Filter the reaction mixture to remove the Raney® nickel. Purify by chromatography on silica gel eluting with DCM/2M ammonia in methanol (9:1) to obtain the title compound (1.5 g, 97%). MS (ES+) m/z: 175 M+H−NH3)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08022062B2 |
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| 출처 데이터셋 | uspto-grants-2011_09 |
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| ORD ID | ord-6c5c2c4d22d44ba9b728fce81a9e5bda |
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| 출처 메모 | uspto-grants-2011_09 |
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