참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Dimethylsulphamoyl chloride | HCID 83372 | — |
| 반응물 | 1H-benzimidazole-2-carbonitrile | HCID 843858 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | Benzimidazole | HCID 5798 | — |
반응 단계
6.2 Grams of a 2-Cyanobenzimidazole compound [compound (iv)]]of the formula (II) in which X is H and Z is OCF2O was dissolved in 100 ml of acetonitrile. 10 Grams of potassium carbonate was added thereto. The resulting mixture was heated under reflux for 15 minutes. Thereafter, 6.7 g of dimethylsulfamoyl chloride was added thereto. Refluxing was continued for 15 minutes with heating. The reaction solution was poured into ice water and extracted with ethyl acetate. The organic layer was washed with water and dried over anhydrous sodium sulfate. Crystals were obtained by removing the solvent from the dried layer by distillation. Recrystallizing the crystals from hexane/ethyl acetate and then from chloroform/methanol gave 2.4 g of benzimidazole derivative [present compound (15)]of the formula (I) in which X is H, Z is OCF2O, R is CN and Q is N(CH3)2.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05310747 |
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| 출처 데이터셋 | uspto-grants-1994_05 |
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| ORD ID | ord-76268cfb746f4a91b4ae0880d81e55de |
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| 출처 메모 | uspto-grants-1994_05 |
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