Thiourea → HCID 11637238、化合物
反応式
Br[CH:2]1[CH2:8][CH2:7][CH2:6][C:5]2[CH:9]=[CH:10][C:11]([F:13])=[CH:12][C:4]=2[C:3]1=O.[NH2:15][C:16]([NH2:18])=[S:17]>C(O)C>[F:13][C:11]1[CH:10]=[CH:9][C:5]2[CH2:6][CH2:7][CH2:8][C:2]3[S:17][C:16]([NH2:18])=[N:15][C:3]=3[C:4]=2[CH:12]=1参加物
4
実験手順
6-Bromo-3-fluoro-6,7,8,9-tetrahydro-5H-benzo[a]cyclohepten-5-one (1.0 g, 3.89 mmole) was mixed with thiourea (355 mg, 4.66 mmole) in 20 ml of ethanol and heated at reflux temperature for 16 hours. The reaction mixture was cooled and filtered to give a solid (m.p. 270° C.). The filtrate was concentrated and then partitioned between ethyl acetate and saturated sodium carbonate solution. The organic extract was concentrated and chromatographed (silica, ethyl acetate/hexanes) to give the desired product as a yellow solid (m.p. 142-144° C., 34%).
後処理
- temperatureheated
- temperatureat reflux temperature for 16 hours
- temperatureThe reaction mixture was cooled
- filtrationfiltered
出典と根拠
- ORDレコード
- ord-c79725920ed84952952c56ea071f48ce
- 出典データセット
- uspto-grants-2007_09
- 特許番号
- US07273880B2
反応ノート
読み込み中…