Sodium Hydroxide → 2-Amino-5-methylbenzenesulfonamide

HRID 2283268노트

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HRID 2283268 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 2455842-Amino-5-methylbenzenesulfonamide수율 85%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

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온도
105 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d82b1a865f21419fb5aee0cd0d4e5618
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09145380B2

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