참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Diethylamine | HCID 8021 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Isobutyl chloroformate | HCID 62365 | — |
| 반응물 | HCID 178482013 | HCID 178482013 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | N,N-diethyl-4-(1-methyl-1,2,3,4-tetrazol-5-yl)thio-butyramide | HCID 21153948 | 57.9% |
반응 단계
3-(1-Methyl-1,2,3,4-tetrazol-5-yl)methylthiopropionic acid (2 g) is dissolved in tetrahydrofuran (50 ml), and thereto is added triethylamine (1.1 g). To the mixture is added dropwise with stirring isobutyl chloroformate (1.5 g) under ice-cooling, and the mixture is stirred at room temperature for 30 minutes. To the mixture is added dropwise with stirring diethylamine (0.9 g) at the same temperature, and the mixture is further stirred for 3 hours. After distilling off the solvent, the resulting residue is subjected to column chromatography (Kieselgel 60, made by Merck & Co., eluting solvent, chloroform:methanol=50:1, V/V) to isolate N,N-diethyl-3-(1-methyl-1,2,3,4-tetrazol-5-yl)methylthio-propionamide (1.5 g), colorless liquid, nD25 =1.5200.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US04663323 |
|---|
| 출처 데이터셋 | uspto-grants-1987_05 |
|---|
| ORD ID | ord-9d670f1263f94423a676f07f0db9da10 |
|---|
| 출처 메모 | uspto-grants-1987_05 |
|---|