反応式
[F:1][C:2]1[CH:3]=[CH:4][C:5]2[S:9]C(C)=[N:7][C:6]=2[CH:11]=1.Cl>C(O)CO.[OH-].[Na+]>[NH2:7][C:6]1[CH:11]=[C:2]([F:1])[CH:3]=[CH:4][C:5]=1[SH:9]参加物
5
反応条件
- 温度
- 129 °C
実験手順
A solution of 5-fluoro-2-methylbenzo[d]thiazole (1.2 g, 7.18 mmol) in ethylene glycol and NaOH (5N, 2 ml) was degassed under N2 for 10 min, then refluxed at 129° C. for 3 hours. The solution was cooled to 0° C. and then acidified to pH 3˜4 using c. HCl. The mixture was extracted with EtOAc (2×50 ml). The organic layer was washed with brine and dried with Na2SO4 and concentrated in vacuo. The crude residue (1.01 g, 98%) was used directly in the next step without purification.
後処理
- temperatureThe solution was cooled to 0° C.
- extractionThe mixture was extracted with EtOAc (2×50 ml)
- washThe organic layer was washed with brine
- dry with materialdried with Na2SO4
- concentrationconcentrated in vacuo
- customThe crude residue (1.01 g, 98%) was used directly in the next step without purification
出典と根拠
- ORDレコード
- ord-017153fa48f5499ca9f2d74947ca74d0
- 出典データセット
- uspto-grants-2016_05
- 特許番号
- US09328067B2
関連ノート
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