참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Citric Acid | HCID 311 | — |
| 반응물 | Triethylethylenediamine | HCID 66040 | — |
| 반응물 | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| 반응물 | 2-(Benzenesulfonyl)ethan-1-amine | HCID 3545497 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | N-[2-(Diethylamino)ethyl]-N-ethyl-N'-[2-(phenylsulfonyl)ethyl]urea citrate | HCID 13655129 | 52% |
반응 단계
A solution of 5.55 g (0.030 mole) of 2-(phenylsulfonyl)ethanamine and 5.35 g (0.033 mole) of 1,1'-carbonyldiimidazole in 400 ml of tetrahydrofuran was stirred at room temperature for 1 hr. A solution of 4.62 g (0.032 mole) of N,N,N'-triethylethylenediamine in 50 ml of tetrahydrofuran was added, and the mixture was refluxed for 16 hr. The solvent was removed in vacuo, and the residue was partitioned between a mixture of 300 ml of methylene chloride and 500 ml of ether and water. The organic phase was dried over magnesium sulfate, and the solvent was removed in vacuo to give an oil. A solution of the oil in methanol was treated with an equivalent of citric acid and ether was added. A white precipitate formed to give 8.54 g (52.0%) of white crystalline solid, m.p. 105°-107° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04724235 |
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| 출처 데이터셋 | uspto-grants-1988_02 |
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| ORD ID | ord-fefe59a7cdf245f1bf02e5ac9fe770f6 |
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| 출처 메모 | uspto-grants-1988_02 |
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