Lawesson's reagent → HCID 53772023, 화합물
반응식
[NH2:1][C:2]([CH2:4][C:5]1[N:9]([CH2:10][C:11]2[CH:18]=[CH:17][C:14]([C:15]#[N:16])=[CH:13][CH:12]=2)[CH:8]=[N:7][CH:6]=1)=O.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:28])=CC=1>O1CCOCC1>[C:15]([C:14]1[CH:17]=[CH:18][C:11]([CH2:10][N:9]2[C:5]([CH2:4][C:2]([NH2:1])=[S:28])=[CH:6][N:7]=[CH:8]2)=[CH:12][CH:13]=1)#[N:16]참가 물질
4
반응 조건
- 온도
- 80 °C
실험 절차
To a 50 mL round bottomed flask with a stirring bar, reflux condenser and an argon inlet was added 4-[5-(aminocarbonyl-methyl)imidazol-1-ylmethyl]benzonitrile (0.36 g, 1.49 mmol), Lawesson's reagent (0.73 g, 1.8 mmol) and 1,4-dioxane (10 mL). This well stirred mixture was heated at 80° C. for 24 hours. The cooled reaction mixture was concentrated in vacuo and the residue was chromatographed (silica gel, 10% 2-propanol in ammonia saturated CHCl3). The title compound was obtained as a yellow, crystalline solid.
후처리
- temperatureTo a 50 mL round bottomed flask with a stirring bar, reflux condenser and an argon inlet
- customThe cooled reaction mixture
- concentrationwas concentrated in vacuo
- customthe residue was chromatographed (silica gel, 10% 2-propanol in ammonia saturated CHCl3)
출처 및 근거
- ORD 기록
- ord-15cd3c0087e7484da76b4d8f04e0b1c8
- 출처 데이터셋
- uspto-grants-1999_02
- 특허 번호
- US05874452
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