1-methyl-1H-indol-5-amine → 5-isothiocyanato-1-methyl-1H-indole
반응식
[NH2:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[N:7]([CH3:11])[CH:6]=[CH:5]2.[C:12](C1NC=CN=1)(C1NC=CN=1)=[S:13]>C(OCC)(=O)C>[N:1]([C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[N:7]([CH3:11])[CH:6]=[CH:5]2)=[C:12]=[S:13]참가 물질
4
반응 조건
- 온도
- 50 °C
실험 절차
A flask was charged with 5-amino-1-methyl-1H-indole (8.8 g; 60 mmol), thiocarbonyl diimidazole (10.7 g; 60 mmol) and ethyl acetate (200 mL). The reaction was heated at 50° C. for five minutes, and after cooling, the solvent was evaporated. The crude material was dissolved in dichloromethane (100 mL) and filtered through a short plug of silica gel, which was washed with another bolus of dichloromethane (100 mL). The organic eluent was evaporated to give 5-isothiocyanato-1-methyl-1H-indole (8.9 g; 47 mmol).
후처리
- temperatureafter cooling
- customthe solvent was evaporated
- dissolutionThe crude material was dissolved in dichloromethane (100 mL)
- filtrationfiltered through a short plug of silica gel, which
- washwas washed with another bolus of dichloromethane (100 mL)
- customThe organic eluent was evaporated
출처 및 근거
- ORD 기록
- ord-863637f6655745558c37dbc39ba37621
- 출처 데이터셋
- uspto-grants-2014_09
- 특허 번호
- US08835464B2
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