Hydrochloric Acid → 3-(N-carbethoxymethyl-N-methylsulfamoyl)-thiophene-2-carboxylic acid methyl ester

HRID 616824

反応式

HRID 616824 の反応式
[CH3:1][O:2][C:3]([C:5]1[S:6][CH:7]=[CH:8][C:9]=1[S:10](Cl)(=[O:12])=[O:11])=[O:4].[CH2:14]([O:16][C:17](=[O:21])[CH2:18][NH:19][CH3:20])[CH3:15].O.Cl>C(Cl)(Cl)Cl>[CH3:1][O:2][C:3]([C:5]1[S:6][CH:7]=[CH:8][C:9]=1[S:10](=[O:12])(=[O:11])[N:19]([CH2:18][C:17]([O:16][CH2:14][CH3:15])=[O:21])[CH3:20])=[O:4]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 95849Glycine, N-methyl-, ethyl esterHCID 27367332-Thiophenecarboxylic acid, 3-(chlorosulfonyl)-, methyl ester

生成物 1

HCID 28087943-(N-carbethoxymethyl-N-methylsulfamoyl)-thiophene-2-carboxylic acid methyl ester

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

20 G. of 3-chlorosulfonylthiophene-2-carboxylic acid methyl ester are dissolved in absolute chloroform, whereupon 21 g. of sarcosine ethyl ester are added dropwise during 10 minutes. In so doing, the mixture warms up to 500° C. After 20 minutes, the mixture is cooled, shaken once each time with water, 0.5-N hydrochloric acid and a sodium bicarbonate solution, dried and evaporated. The remaining oil is brought to crystallization with ethanol. There is obtained 3-(N-carbethoxymethyl-N-methyl-sulfamoyl)-thiophene-2-carboxylic acid methyl ester of melting point 84°-85° C.

後処理

  1. customwarms up to 500° C
  2. temperaturethe mixture is cooled
  3. dry with materiala sodium bicarbonate solution, dried
  4. customevaporated
  5. customThe remaining oil is brought to crystallization with ethanol

出典と根拠

ORDレコード
ord-b6bf8cb5837449b9ab1bb275a5edc885
出典データセット
uspto-grants-1978_02
特許番号
US04076709

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