反応式
[Cl:1][S:2]([C:5]1[CH:9]=[CH:8][S:7][C:6]=1[C:10](Cl)=[O:11])(=[O:4])=[O:3].[CH3:13][OH:14].Cl>C(Cl)(Cl)Cl>[CH3:13][O:14][C:10]([C:6]1[S:7][CH:8]=[CH:9][C:5]=1[S:2]([Cl:1])(=[O:4])=[O:3])=[O:11]参加物
実験手順
48 G. (0.196 mol) of the obtained 3-chlorosulfonylthiophene-2-carboxylic acid chloride are dissolved in 500 ml. of absolute chloroform, 9.6 g. (0.3 mol) of absolute methanol are added and the solution is heated to reflux for 3 hours [until no more hydrogen chloride evolution]. The mixture is evaporated to dryness in vacuo and the residue allowed to crystallize out. There is obtained pure 3-chlorsulfonylthiophene-2-carboxylic acid methyl ester. 2.41 G. (0.010 mol) of the obtained 3-chlorosulfonylthiophene-2-carboxylic acid methyl ester are dispersed together with 1.53 g. of sarcosine ethyl ester hydrochloride in 10 ml. of absolute pyridine and stirred at room temperature. After 2 hours, the mixture is poured on to 50 ml. of ice-cold 2-N hydrochloric acid and extracted five times with 20 ml. of methylene chloride each time. The combined organic phases are dried over sodium sulfate, filtered and evaporated. The crystalline residue is digested with a small amount of ice-cold ethanol.
後処理
- temperaturethe solution is heated
- customThe mixture is evaporated to dryness in vacuo
- customto crystallize out
出典と根拠
- ORDレコード
- ord-ccb1cf14c4f44945b582c0fb637e86e5
- 出典データセット
- uspto-grants-1980_09
- 特許番号
- US04224445
関連ノート
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