Formamide → HCID 178518064、化合物
反応式
[NH2:1][C:2]1[S:3][C:4]2[CH2:15][CH2:14][CH2:13][CH2:12][C:5]=2[C:6]=1[C:7](OCC)=[O:8].[CH:16]([NH2:18])=O>O>[C:5]12[CH2:12][CH2:13][CH2:14][CH2:15][C:4]=1[S:3][C:2]1[N:1]=[CH:16][N:18]=[C:7]([OH:8])[C:6]2=1参加物
4
反応条件
- 温度
- 160 °C
実験手順
Into a 100-mL round-bottom flask containing a solution of ethyl 2-amino-4,5,6,7-tetrahydro-1-benzothiophene-3-carboxylate (4.06 g, 18.02 mmol, 1.00 equiv) in 100 mL of formamide was stirred for 8 h at 160° C. in an oil bath under nitrogen. The reaction mixture was cooled to 0° C. and diluted with water. The solids were filtered and precipitated with ethyl acetate to provide 8-thia-4,6-diazatricyclo[7.4.0.0[2,7]]trideca-1(9),2(7),3,5-tetraen-3-ol (3.0 g, 81%) as a light yellow solid.
後処理
- temperatureThe reaction mixture was cooled to 0° C.
- filtrationThe solids were filtered
- customprecipitated with ethyl acetate
出典と根拠
- ORDレコード
- ord-33c97f8817374f12b694a71b67ed9ed8
- 出典データセット
- uspto-grants-2015_07
- 特許番号
- US09085586B2
反応ノート
読み込み中…