참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Thiourea dioxide | HCID 61274 | — |
| 반응물 | 2-(Hydroxymethyl)-4-methoxy-6-((2-nitrophenyl)diazenyl)phenol | HCID 136348292 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 2-(2H-benzo[d][1,2,3]triazol-2-yl)-6-(hydroxymethyl)-4-methoxyphenol | HCID 66906968 | 20.5% |
반응 단계
In a 500 ml round bottom flask equipped with a magnetic stirrer, regular addition funnel, powder addition funnel, and nitrogen inlet was added 23.6 g (77.7 mmol) 2-(hydroxymethyl)-4-methoxy-6-((2-nitrophenyl)diazenyl)phenol and 200 ml ethanol. NaOH (18.8 g, 470 mmol) was dissolved in 100 ml deionized water and approximately one-fourth was added dropwise to the reaction mixture. The mixture was heated to 80° C. and 25.1 g (232 mmol) formamidine sulfinic acid and the remaining sodium hydroxide solution were concurrently added dropwise to the reaction mixture over 30 minutes. The mixture was stirred at 80° C. for 3 hours, poured into 3.5 L water, and then acidified to pH 4 using 1 N HCl. The resultant solid was collected by filtration and worked up as in Example 5 to give a light yellow solid (4.3 g, 20.5%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08232326B2 |
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| 출처 데이터셋 | uspto-grants-2012_07 |
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| ORD ID | ord-0392a17f1d8d4685b6e04881d046be5f |
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| 출처 메모 | uspto-grants-2012_07 |
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