2,3-Dichlorobenzaldehyde → HCID 15035858、化合物
反応式
[C:1]([O:5][C:6]([N:8]1[CH2:14][C:13](=O)[CH2:12][S:11](=[O:17])(=[O:16])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[Cl:18][C:19]1[C:26]([Cl:27])=[CH:25][CH:24]=[CH:23][C:20]=1[CH:21]=O.[NH2:28]/[C:29](/[CH3:36])=[CH:30]\[C:31]([O:33][CH2:34][CH3:35])=[O:32]>C(O)C>[Cl:18][C:19]1[C:26]([Cl:27])=[CH:25][CH:24]=[CH:23][C:20]=1[CH:21]1[C:12]2[S:11](=[O:17])(=[O:16])[CH2:10][CH2:9][N:8]([C:6]([O:5][C:1]([CH3:4])([CH3:3])[CH3:2])=[O:7])[CH2:14][C:13]=2[NH:28][C:29]([CH3:36])=[C:30]1[C:31]([O:33][CH2:34][CH3:35])=[O:32]参加物
5
実験手順
A mixture of 4-N-(t-butyloxycarbonyl)-1,1-dioxo -2,3,4,5,6,7-hexahydro-1,4-thiazepin-6-one (2.00 g, 7.60 mmole) from Example 6, 2,3-dichlorobenzaldehyde (1.33 g, 7.60 mmole) and ethyl 3-aminocrotonate (0.98 g, 7.60 mmole) was heated to reflux in 40 mL of ethanol for 24 hours. The ethanol was removed under reduced pressure and replaced with 85 mL of toluene. The mixture was heated to reflux for 2 hours, cooled to room temperature and filtered to obtain the produce (2.45 g, 61%).
後処理
- temperaturewas heated
- customThe ethanol was removed under reduced pressure
- temperatureThe mixture was heated
- temperatureto reflux for 2 hours
- filtrationfiltered
- customto obtain the
- customproduce (2.45 g, 61%)
出典と根拠
- ORDレコード
- ord-06de9772ec26415da65775a0f59258d3
- 出典データセット
- uspto-grants-1991_12
- 特許番号
- US05075440
反応ノート
読み込み中…