참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Acetate | HCID 517045 | — |
| 반응물 | 3-Methyl-2-(3-sulfopropylthio) benzothiazolium hydroxide | HCID 86735756 | — |
| 반응물 | HCID 178478652 | HCID 178478652 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | HCID 178481663 | HCID 178481663 | 98.7% |
반응 단계
175 g of anhydrous 3-methyl-2-(3-sulfopropylthio) benzothiazolium hydroxide was added to a mixture of 100 g of 5-aminobenzotriazole di-hydrochloride, 120 g of sodium acetate and 1000 ml of water under heating at 50° C with stirring in a 2000 ml flask. After stirring for 1 hour at 85° C the mixture was cooled (15° C) with water. The precipitate formed was collected by filtration, washed with water and then with acetonitrile to yield 135 g of crystals. These crystals were dissolved by heating (90° C) in 350 ml of dimethylformamide and the solution was treated with active carbon and filtered. By addition of 1400 ml of acetonitrile to the filtrate, crystals were formed. The crystals were collected to yield 121 g of the desired compound. The melting point was 240.5° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04095984 |
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| 출처 데이터셋 | uspto-grants-1978_06 |
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| ORD ID | ord-83e9387fa1c541aeaaebcb2cb3c4802e |
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| 출처 메모 | uspto-grants-1978_06 |
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