Ammonia → 5-Phenylsulphonyl-6-methyl-1,3-benzodioxole-2-carboxylic acid amide

HRID 745808ノート

反応式

HRID 745808 の反応式
C([O:3][C:4]([CH:6]1[O:10][C:9]2[CH:11]=[C:12]([CH3:24])[C:13]([S:15]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)(=[O:17])=[O:16])=[CH:14][C:8]=2[O:7]1)=O)C.[NH3:25]>O1CCOCC1>[C:18]1([S:15]([C:13]2[C:12]([CH3:24])=[CH:11][C:9]3[O:10][CH:6]([C:4]([NH2:25])=[O:3])[O:7][C:8]=3[CH:14]=2)(=[O:17])=[O:16])[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

参加物

4

反応物 2

HCID 222AmmoniaHCID 539637605-Methyl-6-phenylsulphonyl-1,3-benzodioxole-2-carboxylic acid ethyl ester

生成物 1

HCID 543307335-Phenylsulphonyl-6-methyl-1,3-benzodioxole-2-carboxylic acid amide

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

34.8 g (0.1 mol) of 5-phenylsulphonyl-6-methyl-1,3-benzodioxole-2-carboxylic acid ethyl ester (from Example 2) are dissolved in 350 ml of dioxan (absolute) and treated in a pressure autoclave with approximately 20 g of ammonia gas. The reaction mixture is heated for 10 hours at 80° in the autoclave, the pressure is released, and the solution is concentrated to dryness by evaporation under reduced pressure. The residue is recrystallised from 120 ml of ethanol, yielding colourless crystals of 5-phenylsulphonyl-6-methyl-1,3-benzodioxole-2-carboxylic acid amide having a melting point of 138°-141°.

後処理

  1. temperatureThe reaction mixture is heated for 10 hours at 80° in the autoclave
  2. concentrationthe solution is concentrated to dryness by evaporation under reduced pressure
  3. customThe residue is recrystallised from 120 ml of ethanol

出典と根拠

ORDレコード
ord-034e0728bad14461940e12d8a25db720
出典データセット
uspto-grants-1986_07
特許番号
US04600709

反応ノート

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