Methylamine → methyl 3-(N-methylsulfamoyl)thiophene-2-carboxylate

HRID 59734

反応式

HRID 59734 の反応式
Cl[S:2]([C:5]1[CH:9]=[CH:8][S:7][C:6]=1[C:10]([O:12][CH3:13])=[O:11])(=[O:4])=[O:3].C1COCC1.[CH3:19][NH2:20]>C(Cl)Cl>[CH3:19][NH:20][S:2]([C:5]1[CH:9]=[CH:8][S:7][C:6]=1[C:10]([O:12][CH3:13])=[O:11])(=[O:4])=[O:3]

参加物

5

反応物 3

HCID 6329MethylamineHCID 8028TetrahydrofuranHCID 27367332-Thiophenecarboxylic acid, 3-(chlorosulfonyl)-, methyl ester

生成物 1

HCID 12906749methyl 3-(N-methylsulfamoyl)thiophene-2-carboxylate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of methyl 3-(chlorosulfonyl)thiophene-2-carboxylate (500 mg, 2.077 mmol) in DCM (20 ml), methanamine 2N solution in THF (4.155 ml, 8.31 mmol) was added and the reaction was stirred for 1 hour at RT. The mixture was partitioned between 2N HCl and DCM and the aqueous phase was extracted with DCM. The combined organic layers were dried over sodium sulfate and the solvent was removed affording methyl 3-(N-methylsulfamoyl)thiophene-2-carboxylate (Int. 32) (430 mg, 1.828 mmol, MS/ESI+235.8 [MH]+).

後処理

  1. customThe mixture was partitioned between 2N HCl and DCM
  2. extractionthe aqueous phase was extracted with DCM
  3. dry with materialThe combined organic layers were dried over sodium sulfate
  4. customthe solvent was removed

出典と根拠

ORDレコード
ord-9b66d920a79c456da03aea4e17f10758
出典データセット
uspto-grants-2016_09
特許番号
US09440954B2

関連ノート

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