참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1,3-Dichloroacetone | HCID 10793 | — |
| 반응물 | 3-Chloropropionitrile | HCID 10963 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Thiourea | HCID 2723790 | — |
| 반응물 | Amidinothiourea | HCID 2724563 | — |
| 용매 | Acetone | HCID 180 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Isopropanol | HCID 3776 | — |
| 생성물 | HCID 178511217 | HCID 178511217 | 61.1% |
반응 단계
Into a 500 mL round bottom flask equipped with an overhead stirrer and under an inert atmosphere was added 25 g of 1,3-dichloroacetone (0.197 mol) and 75 g of acetone. The reaction mixture was cooled to 10° C. and 23.2 g 2-imino-4-thiobiuret (0.197 mol) was added. The reaction mixture was stirred for one hour at 10 C. The reaction mixture was then heated to 40° C. and 15 g of thiourea (0.197 mol) was added, followed by the addition of 100 g of water. The mixture was heated to and held at 52° C. for one hour. Acetone was then removed by vacuum distillation. To the reaction mixture was added 100 g of water, 17 g of 3-chloropropionitrile (0.190 mol) and 40 g of isopropyl alcohol. The reaction mixture was cooled below 10° C. and 25 g of an aqueous solution of sodium hydroxide (80 g water) was added dropwise maintaining the reaction temperature below 10° C. The reaction mixture was for 2 hours, filtered and washed to produce 28 g of N-[4-(cyanoethylthiomethyl)-2-thiazolyl]guanidine product.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05856500 |
|---|
| 출처 데이터셋 | uspto-grants-1999_01 |
|---|
| ORD ID | ord-f3466171283b4e8baa7b035687e671be |
|---|
| 출처 메모 | uspto-grants-1999_01 |
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