Ammonia → 3-Thiophenecarboxylic acid, 4-(aminosulfonyl)-, methyl ester

HRID 436828ノート

反応式

HRID 436828 の反応式
Cl[S:2]([C:5]1[C:6]([C:10]([O:12][CH3:13])=[O:11])=[CH:7][S:8][CH:9]=1)(=[O:4])=[O:3].[NH3:14]>C(Cl)(Cl)Cl>[S:2]([C:5]1[C:6]([C:10]([O:12][CH3:13])=[O:11])=[CH:7][S:8][CH:9]=1)(=[O:4])(=[O:3])[NH2:14]

参加物

4

反応物 2

HCID 222AmmoniaHCID 12593671Methyl 4-(chlorosulfonyl)thiophene-3-carboxylate

生成物 1

HCID 30422843-Thiophenecarboxylic acid, 4-(aminosulfonyl)-, methyl ester

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

39.9 g (0.166 mole) of methyl 4-chlorosulfonylthiophene-3-carboxylate (VIII) is dissolved in 400 ml of absolute chloroform; ammonia is passed in at room temperature until the mixture has an alkaline reaction. After the mixture has been stirred for a further 3 hours (care being taken that the solution remains alkaline) it is extracted with water and the organic phase is dried and evaporated. The crystalline residue can be recrystallized from ethanol; however, for further use, digestion with ether is sufficient.

後処理

  1. customis passed in at room temperature until the mixture
  2. customan alkaline reaction
  3. extractionis extracted with water
  4. customthe organic phase is dried
  5. customevaporated
  6. customThe crystalline residue can be recrystallized from ethanol

出典と根拠

ORDレコード
ord-ea5cf465562c4a609d34e2c35fc2658b
出典データセット
uspto-grants-1977_06
特許番号
US04028373

反応ノート

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