Sodium Hydroxide → 2-Amino-5-methylbenzenesulfonamide

HRID 2283268ノート

反応式

HRID 2283268 の反応式
[CH3:1][C:2]1[CH:14]=[CH:13][C:5]2[NH:6]C(=O)[NH:8][S:9](=[O:11])(=[O:10])[C:4]=2[CH:3]=1.[OH-].[Na+]>OS(O)(=O)=O>[NH2:6][C:5]1[CH:13]=[CH:14][C:2]([CH3:1])=[CH:3][C:4]=1[S:9]([NH2:8])(=[O:10])=[O:11]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 100818972H-1,2,4-Benzothiadiazin-3(4H)-one, 7-methyl-, 1,1-dioxide

生成物 1

HCID 2455842-Amino-5-methylbenzenesulfonamide収率 85%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

反応条件

温度
105 °C

実験手順

A mixture of 7-methyl-1,1-dioxo-1,4-dihydro-2-H-benzo[1,2,4]thiadiazin-3-one (7.20 g, 36.36 mmol) in aqueous H2SO4 (50% v/v, 200 mL) was heated at 105° C. for 16 h. The clear solution was then cooled to 0° C. and neutralized using 5N NaOH. The product was extracted with ethyl acetate. The combined extracts were washed with water and concentrated under reduced pressure. The crude product was purified by flash column chromatography using ethyl acetate/hexane (1:1) to afford 4.5 g (85%) of the title compound.

後処理

  1. temperatureThe clear solution was then cooled to 0° C.
  2. extractionThe product was extracted with ethyl acetate
  3. washThe combined extracts were washed with water
  4. concentrationconcentrated under reduced pressure
  5. customThe crude product was purified by flash column chromatography

出典と根拠

ORDレコード
ord-d82b1a865f21419fb5aee0cd0d4e5618
出典データセット
uspto-grants-2015_09
特許番号
US09145380B2

反応ノート

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