참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Carbon Dioxide | HCID 280 | — |
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | 1,2-Phenylenediamine dihydrochloride | HCID 11990 | — |
| 반응물 | 2-(Tert-butyl)pyrimidine-5-carbonitrile | HCID 817771 | — |
| 반응물 | 3,4-Diamino-6-tert-butylpyridine dihydrochloride | HCID 67995003 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | HCID 67995414 | HCID 67995414 | — |
반응 단계
Preparation analogous to 16), S43, using 16.1 g (100 mmol) of 2-tert-butyl-5-cyanopyrimidine [126230-72-6] and 71.4 g (300 mmol) of 3,4-diamino-6-tert-butylpyridine dihydrochloride (S50) instead of 25.9 g (100 mmol) of 2-N-pivaloylamido-3-cyano-6-tert-butylpyridine (S42) and 90.5 g (500 mmol) of o-phenylenediamine dihydrochloride [615-28-1]. After cooling, the violet melt is dissolved in a mixture of 150 ml of ethanol and 300 ml of water at elevated temperature, and a solution of 25 g of sodium carbonate in 100 ml of water is then added dropwise with vigorous stirring (note: foaming, evolution of carbon dioxide). When the addition is complete, the mixture is stirred for a further 30 min., the brown solid is then filtered off with suction, washed three times with 100 ml of water each time and dried in vacuo. Yield: 23.8 g (77 mmol), 77%. Purity: >95% according to 1H-NMR.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09273080B2 |
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| 출처 데이터셋 | uspto-grants-2016_03 |
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| ORD ID | ord-5e49d604c9bd434f8499cee66314e496 |
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| 출처 메모 | uspto-grants-2016_03 |
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