HCID 58545553、化合物 → HCID 58545574、化合物
反応式
CON(C)[C:4]([C:6]1[S:10][CH:9]2[CH:11]=[CH:12][S:13][CH:8]2[CH:7]=1)=[O:5].[CH3:15][Mg]Br>C1COCC1>[S:10]1[C:6]([C:4](=[O:5])[CH3:15])=[CH:7][CH:8]2[S:13][CH:12]=[CH:11][CH:9]12参加物
4
実験手順
3a,6a-Dihydro-thieno[3,2-b]thiophene-2-carboxylic acid methoxy-methyl-amide (1.955 g, 8.60 mmol) was dissolved in THF. The stirred solution was cooled to 0° C. before methylmagnesium bromide (1.4 M in PhMe, 8.6 mL, 12.04 mmol) was added. The reaction was allowed to gradually warm to RT o/n, then it was quenched by addition of 10% HCl. The aqueous phase was extracted with diethyl ether. The organic phase was washed with brine then dried over MgSO4, filtered and concentrated to afford the title compound (1.98 g, 80%).
後処理
- additionwas added
- customwas quenched by addition of 10% HCl
- extractionThe aqueous phase was extracted with diethyl ether
- washThe organic phase was washed with brine
- dry with materialthen dried over MgSO4
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-47dd8055b5d549b4a287e9bd0d63a363
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08822430B2
反応ノート
読み込み中…