참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetaldehyde | HCID 177 | — |
| 반응물 | 3,5-Dibromo-1-methyl-1H-1,2,4-triazole | HCID 17186052 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 1-(3-Bromo-1-methyl-1H-1,2,4-triazol-5-YL)ethan-1-OL | HCID 90017669 | 73% |
반응 단계
To a solution of 3,5-dibromo-1-methyl-1H-1,2,4-triazole (2.634 g, 10.9 mmol, Eq: 1.00) in tetrahydrofuran (184 ml) was added dropwise at −78° C. under argon atmosphere n-butyllithium 1.6 M in hexanes (6.83 ml, 10.9 mmol, Eq: 1.00). The resulting mixture was stirred for 20 minutes at −75° C. then a solution of acetaldehyde (1.2 g, 1.54 ml, 27.3 mmol, Eq: 2.5) in tetrahydrofuran (36.9 ml) was added slowly and stirring at −75° C. was continued for further 1.5 hours. The mixture was quenched with sat. aq. NH4Cl solution and was warmed to 25° C. The mixture was diluted with ethyl acetate and washed 2 times with water. The organic layer was separated, dried over magnesium sulfate, filtrated and evaporated affording 1-(5-bromo-2-methyl-2H-[1,2,4]triazol-3-yl)-ethanol (1.639 g, 72.7%) as a light yellow oil. MS: m/z=206209 (M+H+)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09394311B2 |
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| 출처 데이터셋 | uspto-grants-2016_07 |
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| ORD ID | ord-dbe8a30ef8e54d02817cca29a94c5b94 |
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| 출처 메모 | uspto-grants-2016_07 |
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