Methanol → 2-Aminothiophene-3-carboxamide
반응식
O[CH:2]1[CH2:7]SC(O)C[S:3]1.[C:9]([CH2:11][C:12]([NH2:14])=[O:13])#[N:10].CO>O.C(N(CC)CC)C>[NH2:10][C:9]1[S:3][CH:2]=[CH:7][C:11]=1[C:12]([NH2:14])=[O:13]참가 물질
6
반응 조건
- 온도
- 37.5 °C
실험 절차
2,5-Dihydroxy-1,4-dithiane (76 g) and cyanoacetamide (84 g) were added to a mixture of methanol (180 mL), water (10 mL) and triethylamine (10 g). The resulting mixture was heated at 35-40° C. for about 30 minutes while stirring, and then heated to 50-60° C. for an additional 30 minutes with stirring. The reaction mixture was then cooled to room temperature and poured into a mixture of ice (100 g)/water (360 mL). A fine precipitate formed upon addition, which was filtered and dried overnight to give 100.6 g of the title compound as a pale gray powder ((M+H)+=143, M.P.=159.0-159.6° C.).
후처리
- temperatureheated to 50-60° C. for an additional 30 minutes
- stirringwith stirring
- temperatureThe reaction mixture was then cooled to room temperature
- customA fine precipitate formed upon addition, which
- filtrationwas filtered
- customdried overnight
출처 및 근거
- ORD 기록
- ord-935fc3f083c445918b8be8fdace31fac
- 출처 데이터셋
- uspto-grants-2008_11
- 특허 번호
- US07449472B2
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