Hydrochloric Acid → 2-Thiophenecarboxylic acid, 3-(chlorosulfonyl)-, methyl ester

HRID 28008

반응식

HRID 28008 반응식
[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]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 13755631HCID 13755631, 화합물

생성물 1

HCID 27367332-Thiophenecarboxylic acid, 3-(chlorosulfonyl)-, methyl ester

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

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.

후처리

  1. temperaturethe solution is heated
  2. customThe mixture is evaporated to dryness in vacuo
  3. customto crystallize out

출처 및 근거

ORD 기록
ord-ccb1cf14c4f44945b582c0fb637e86e5
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04224445

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