참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 4-Nitrobenzylamine | HCID 29147 | — |
| 반응물 | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| 반응물 | 3-(tert-Butoxycarbonyl)-1,3-thiazolidine-2-carboxylic acid | HCID 4644094 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | N-(4-nitrobenzyl)-3-(t-butoxycarbonyl)thiazolidine-2-carboxamide | HCID 21918695 | 80% |
반응 단계
3-(t-butoxycarbonyl)thiazolidine-2-carboxylic acid (1 g, 4.3 mmol) and carbonyldiimidazole (0.7 g, 4.3 mmol) are dissolved in THF (10 ml). the mixture is agitated for 1 hour at ambient temperature. 4-nitrobenzylamine (0.81 g, 4.3 mmoles) and triethylamine (0.6 ml. 0.43 g, 4.3 mmoles) in suspension in 10 ml of a THF and DMF mixture (1/1) are added to the preceding solution and the whole is heated under reflux for 5 hours. The solvents are then evaporated off under reduced pressure. The residue is taken up in 25 ml of ethyl acetate and washed 3 times with 15 ml of water. The organic phase is dried and the solvent is evaporated off under reduced pressure. The product obtained is purified on silica gel in a dichloromethane/methanol mixture (95/5). N-(4-nitrobenzyl)-3-(t-butoxycarbonyl)thiazolidine-2-carboxamide is obtained in the form of a pale yellow oil with a yield of 80% (1.25 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US06630461B2 |
|---|
| 출처 데이터셋 | uspto-grants-2003_10 |
|---|
| ORD ID | ord-84801aee34014f70ac9484def1a8ad64 |
|---|
| 출처 메모 | uspto-grants-2003_10 |
|---|