참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Bromoacetyl bromide | HCID 61147 | — |
| 반응물 | 1-Pyrenemethanol | HCID 104977 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | Pyren-1-ylmethyl 2-bromoacetate | HCID 15686801 | 100.6% |
반응 단계
Pyrenemethanol (Pyr-OH) (109.6 mg, 0.47 mmol) in 1.0 mL DMF (anh) was treated with 180 μL TEA (anh, 1.29 mmol) and 2-bromoacetyl bromide (132.2 μL, 1.50 mmol) in 1 mL dichloromethane. The mixture was stirred at RT (˜23° C.) for 17 hours. After the solvent was evaporated, the crude product was purified by silica gel column (Hex/EtOAc=2/1) to give 167 mg final product as a yellow solid (yield 90%). 1H NMR (CDCl3, 500 MHz): δ 8.28-8.03 (m, 9H, ArH), 5.94 (s, 2H, ArCH2), 3.90 (s, 2H, CH2Br). ESI: 375, [M+Na]+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09028880B2 |
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| 출처 데이터셋 | uspto-grants-2015_05 |
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| ORD ID | ord-1f6638ac4c364df394bacf3e07c31fe7 |
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| 출처 메모 | uspto-grants-2015_05 |
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