反応式
[NH2:1][NH:2][C:3]([NH2:5])=[S:4].[Cl:6][C:7]1[CH:8]=[C:9]([CH2:14][C:15](Br)=O)[CH:10]=[CH:11][C:12]=1[Cl:13]>O1CCOCC1>[Cl:6][C:7]1[CH:8]=[C:9]([C:14]2[N:5]=[C:3]([NH:2][NH2:1])[S:4][CH:15]=2)[CH:10]=[CH:11][C:12]=1[Cl:13]参加物
4
実験手順
A solution of a thiosemicarbazide (10 mmol, 0.91 g) and 3,4-dichlorophenylacetyl bromide (10 mmol, 2.68 g) in dioxane (20 mL) was stirred at room temperature for 16 h. The precipitate of hydrobromide salt was filtered and washed with dioxane (3×10 mL), then basified with 2N Na2CO3 (20 mL). The product was filtered, washed with water and dried (2.08 g, 80%). The product was generally satisfactory for further reaction.
後処理
- filtrationThe precipitate of hydrobromide salt was filtered
- washwashed with dioxane (3×10 mL)
- filtrationThe product was filtered
- washwashed with water
- customdried (2.08 g, 80%)
- customThe product was generally satisfactory for further reaction
出典と根拠
- ORDレコード
- ord-fafdaf905cb64141b0acd6ca0cc5b18e
- 出典データセット
- uspto-grants-2012_09
- 特許番号
- US08257931B2
関連ノート
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