참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Aluminium lithium hydride | HCID 21226445 | — |
| 반응물 | tert-butyl N-[2-(morpholin-4-yl)ethyl]carbamate | HCID 58930414 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | Methyl(2-(morpholin-4-yl)ethyl)amine | HCID 14979282 | — |
반응 단계
Into a 250-mL 3-necked round-bottom flask, was placed a solution of LiAlH4 (7.72 g, 208.65 mmol, 3.00 equiv) in tetrahydrofuran (60 mL). This was followed by the addition of a solution of tert-butyl 2-morpholinoethylcarbamate (16 g, 62.61 mmol, 1.00 equiv, 90%) in tetrahydrofuran (40 mL) dropwise with stirring at 0-5° C. The resulting solution was stirred for 2 h at 70° C. in a oil bath. The reaction was then quenched by the addition of 7.7 mL of water, 7.7 mL of 15% sodium hydroxide, and 23.1 mL of water. The solids were filtered out. The mixture was dried over sodium sulfate and concentrated under vacuum. The residue was applied onto a silica gel column and eluted with dichloromethane:methanol (0.5% triethylamine) (20:1). This resulted in 4.2 g (42%) of N-methyl-2-morpholinoethanamine as brown oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09301951B2 |
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| 출처 데이터셋 | uspto-grants-2016_04 |
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| ORD ID | ord-16d1fdfc315f499c8a3fd13ad2779efa |
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| 출처 메모 | uspto-grants-2016_04 |
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