Oxalyl chloride → HCID 73446015、化合物
反応式
[C:1](Cl)(=O)[C:2]([Cl:4])=[O:3].[K+].[C:8]([C:10]([C:15]1[S:16][CH:17]=[CH:18][CH:19]=1)=CC([O-])=O)#[N:9]>C(Cl)Cl>[C:8]([C:10]([C:15]1[S:16][CH:17]=[CH:18][CH:19]=1)=[CH:1][C:2]([Cl:4])=[O:3])#[N:9]参加物
4
実験手順
To a stirring solution of oxalyl chloride (81.17 mL, 0.93 mol) in CH2Cl2 (350 mL) was added 3-cyano-3-thiophen-2-yl-acrylic acid potassium salt 21 (100 g, 0.45 mol) portion-wise over 20 min. An additional 250 mL of CH2Cl2 were added to assist stirring. The slurry was stirred at room temperature for 30 min and was then filtered. The potassium chloride salts were washed with copious CH2Cl2. Collected organic rinses were combined and solvent removed under vacuum to afford 84.3 g of 22, which was carried on to the next step without further purification.
後処理
- stirringThe slurry was stirred at room temperature for 30 min
- filtrationwas then filtered
- washThe potassium chloride salts were washed with copious CH2Cl2
- customsolvent removed under vacuum
出典と根拠
- ORDレコード
- ord-2f8534574f344b848fdc6f33cbfe4136
- 出典データセット
- uspto-grants-2009_12
- 特許番号
- US07635695B2
反応ノート
読み込み中…