Hydrochloric Acid → 2H,3H-1lambda6-thieno[2,3-d][1,2]thiazole-1,1,3-trione

HRID 2212238ノート

反応式

HRID 2212238 の反応式
[S:1]([C:5]1[C:6](C(OC)=O)=[CH:7][S:8][CH:9]=1)(=[O:4])(=[O:3])[NH2:2].[CH3:14][O-:15].[Na+].Cl>CO>[O:4]=[S:1]1(=[O:3])[C:5]2[CH:6]=[CH:7][S:8][C:9]=2[C:14](=[O:15])[NH:2]1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 30422843-Thiophenecarboxylic acid, 4-(aminosulfonyl)-, methyl esterHCID 10942334Sodium Methoxide

生成物 1

HCID 140865502H,3H-1lambda6-thieno[2,3-d][1,2]thiazole-1,1,3-trione

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of methyl 4-sulfamoylthiophene-3-carboxylate (2.7 g, 12.2 mmol), methanol (12 mL), and a 25% methanolic solution of sodium methylate (3.6 mL) was refluxed for 48 h. The reaction mixture was cooled to room temperature and acidified with concentrated hydrochloride acid, and the precipitated product was collected and washed with water. Recrystallized from water, yielded 400 mg of the title compound. MS: 187.8 (M−1), 189.5 (M+1). 1H NMR (DMSO-d6): 8.34 (d, J=4.4 Hz, 1H), 7.705 (d, J=4.8 Hz, 1H).

後処理

  1. customthe precipitated product was collected
  2. washwashed with water
  3. customRecrystallized from water

出典と根拠

ORDレコード
ord-7b537e2b0847459fa2f532f5b070956c
出典データセット
uspto-grants-2006_09
特許番号
US07101880B2

反応ノート

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