참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Potassium Iodide | HCID 4875 | — |
| 반응물 | 2-Imidazolidinone | HCID 8453 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 2-Hydroxy-5-nitrobenzyl bromide | HCID 13044 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 1-(2-Hydroxy-5-nitrobenzyl)-2-imidazolidinone | HCID 13006892 | — |
반응 단계
A 7.9 g (0.092 mole) portion of 2-imidazolidinone in 92 ml of dimethylsulfoxide was treated with 12.7 g (0.092 mole) of K2CO3, 7.4 g (0.045 mole) of potassium iodide and 20.0 g (0.092 mole) of 2-hydroxy-5-nitrobenzyl bromide. The reaction mixture was heated to 105° over 0.3 hours and held at 105° for 1.6 hours. The reaction mixture was poured with stirring into 550 ml of water. The aqueous mixture was acidified with 9 ml of concentrated HCl and extracted with 480 ml of chloroform. The chloroform extract was washed with 60 ml of H2O, dried over MgSO4 overnight and filtered. The filtrate was concentrated under reduced pressure to give 18 g of a yellow semi-solid. The crude product was crystallized using 65 ml of benzene and filtered, washing with ether to give 9.7 g (44%) of a light yellow semi-solid. Recrystallization from acetonitrile gave an analytical sample, m.p. 222°-224° dec.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US03932452 |
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| 출처 데이터셋 | uspto-grants-1976_01 |
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| ORD ID | ord-68b133b975dd448389ab1c8fc39c6058 |
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| 출처 메모 | uspto-grants-1976_01 |
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