Formamide → HCID 135957237、化合物
反応式
[NH2:1][C:2]1[CH:12]=[CH:11][C:5]2[S:6](=[O:10])(=[O:9])[CH2:7][CH2:8][C:4]=2[C:3]=1[C:13]([OH:15])=O.[CH:16]([NH2:18])=O.O>CN(C)C=O>[O:9]=[S:6]1(=[O:10])[C:5]2=[CH:11][CH:12]=[C:2]3[C:3]([C:13](=[O:15])[NH:18][CH:16]=[N:1]3)=[C:4]2[CH2:8][CH2:7]1参加物
5
実験手順
0.87 g (3.83 mmol) of 5-amino-1,1-dioxo-2,3-dihydro-1H-1λ6-benzo[b]-thiophene-4-carboxylic acid was suspended in 2.0 ml of N,N-dimethyl-formamide and, after addition of 0.76 ml (19.14 mmol) of formamide, reacted in a microwave at 150° C. and 60 W for 40 min. During the reaction, the pressure in the microwave rose to 20 bar. The reaction mixture was then added to water. The precipitated solid was filtered off with suction and washed successively with water and diethyl ether and dried in vacuo overnight. 440 mg of the desired compound were obtained.
後処理
- customreacted in a microwave at 150° C.
- customDuring the reaction
- filtrationThe precipitated solid was filtered off with suction
- washwashed successively with water and diethyl ether
- customdried in vacuo overnight
出典と根拠
- ORDレコード
- ord-cececc1be3b44a75bbe302f258543598
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07741333B2
反応ノート
読み込み中…