참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Diethylthiocarbamoyl chloride | HCID 66607 | — |
| 반응물 | 2(1H)-Pyrimidinone, tetrahydro-1,3-dimethyl- | HCID 81646 | — |
| 반응물 | N,N-diethyl-3-hydroxypyridine-2-carboxamide | HCID 3020810 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | N,N-diethyl-3-(N',N'-diethylthiocarbamoyloxy)picolinamide | HCID 19963243 | 83% |
반응 단계
258.3 g (1.33 mol) of 3-hydroxy-N,N-diethylpicolinamide are introduced into 1 l of dimethylpropyleneurea and 213.2 ml (1.53 mol) of triethylamine at 0° C., and 222 g (1.464 mol) of diethylthiocarbamoyl chloride are introduced in the form of a solid. After the reaction mixture has been stirred for 2 hours at 0° C., it is poured into 2 l of water and extracted three times using ethyl acetate, the ethyl acetate phases are washed five times using 500 ml of water in each case, and the combined organic phases are dried over Na2SO4 and concentrated in vacuo at 60° C. Recrystallization from Et2O/hexane gives 341 g (83%) of brown crystals, m.p. 70°-72° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05616590 |
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| 출처 데이터셋 | uspto-grants-1997_04 |
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| ORD ID | ord-7f4daed40d314eedb8125aa00e940a83 |
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| 출처 메모 | uspto-grants-1997_04 |
|---|