참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methoxyacetic Acid | HCID 12251 | — |
| 반응물 | Phosphorus oxychloride | HCID 24813 | — |
| 반응물 | Thiosemicarbazide | HCID 2723789 | — |
| 반응물 | Sodium | HCID 5360545 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 5-(Methoxymethyl)-1,3,4-thiadiazol-2-amine | HCID 660844 | 81% |
반응 단계
To a suspension of thiosemicarbazide a24 (40 g, 0.44 mol, 1 eq) in dioxane (400 ml) at room temperature is added methoxyacetic acid (39.56 g, 0.44 mol, 1 eq) in one portion, and the reaction mixture is heated at 80° C. then phosphorous oxychloride (67.54 g, 0.44 mol, 1 eq) is carefully added over 1.5 hours. After reaction completion (4 hours), water is added and the solution is neutralised to pH=6-7 with sodium hydroxyde pellets. After extraction EtOAc/iPrOH (9/1) and evaporation under vacuum, the residue is recrystallized from MeTHF/iPrOH to afford 51 g of pure 5-(methoxymethyl)-1,3,4-thiadiazol-2-amine a25.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08822508B2 |
|---|
| 출처 데이터셋 | uspto-grants-2014_09 |
|---|
| ORD ID | ord-06c0c059141a44578f5004c4a2aa0a42 |
|---|
| 출처 메모 | uspto-grants-2014_09 |
|---|
