참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Bromide | HCID 253877 | — |
| 반응물 | Sodium Methoxide | HCID 10942334 | — |
| 반응물 | 1,2-Dibromo-1,2-di(4-bromobenzoyl)ethane | HCID 11731356 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 1,2-Bis(4-bromobenzoyl)-1-methoxyethane | HCID 19693491 | — |
반응 단계
To a solution of 1,2-dibromo-1,2-di(4-bromobenzoyl) ethane (11.1 g, 0.02 mole) in 150 mL dry methanol was added a solution of sodium methoxide in methanol (0.92 g sodium in 50 mL methanol). The yellow brown mixture was refluxed for 1-1.5 hr. The solvent was removed by distillation, the residue was suspended in water and the mixture was extracted with 100 mL chloroform. The chloroform extract was washed with water, dried (Na2SO4) and concentrated. The residue obtained was titrated with dry methanol-ether (3:1) to yield off-white crystalline solid, 6.6 g (78%), mp 153°-154° C. IR (KBr): 3106, 3062, 2932, 1689, 1649, 1583, 1556, 1403, 1223, 1202, 1182, 1086, 1010, 1000, 857, 814, 738, 618, 472 cm-1. 1H (DMSO-d6 /40° C.): 7.95 (d, 2H, J=7.8), 7.77 (4H, J=8.8), 7.72 (d, 2H, J=7.8), 6.89 (s, 1H), 4.03 (s, 3H). 13C (DMSO-d6 /40° C.): 189.9, 187.2, 168.8, 139.9, 135.9, 133.1, 132.2, 131.8, 130.3, 128.1, 127.4, 98.6, 58.5. MS m/e 424 (M+).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05723288 |
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| 출처 데이터셋 | uspto-grants-1998_03 |
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| ORD ID | ord-68a4112e542d4a8cb9aa4b70a263e0cb |
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| 출처 메모 | uspto-grants-1998_03 |
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