Hydrochloric Acid → 4-Methyl-5-iodosaccharin

HRID 343749

반응식

HRID 343749 반응식
Cl.[CH3:2][C:3]1[C:8]2[C:9](=[O:14])[NH:10][S:11](=[O:13])(=[O:12])[C:7]=2[CH:6]=[CH:5][C:4]=1N.N([O-])=O.[Na+].[I-:20].[K+]>O.C(O)(=O)C>[CH3:2][C:3]1[C:8]2[C:9](=[O:14])[NH:10][S:11](=[O:13])(=[O:12])[C:7]=2[CH:6]=[CH:5][C:4]=1[I:20]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 4875Potassium IodideHCID 23668193Sodium NitriteHCID 701876914-Methyl-5-aminosaccharin

생성물 1

HCID 153462934-Methyl-5-iodosaccharin

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매2회

반응 조건

온도
50 °C

실험 절차

A mixture of 205 ml of glacial acetic acid, 160 ml of water and 40 ml of conc. HCl is initially taken and 23.4 g (0.11 mol) of 4-methyl-5-amino-1,1,3-trioxo-2,3-dihydro-1λ6 benz[d]isothiazole are introduced with stirring at 15°-20° C. 7.9 g (0.115 mol) of sodium nitrite are added dropwise to the resulting suspension at 5°-10° C. and it is stirred at 5° C. for 30 min. The diazonium salt, which is present as a suspension, is then added dropwise in portions to a solution of 19.1 g (0.115 mol) of potassium iodide in 170 ml of water which is warmed to 50° C., nitrogen being formed. After cooling to room temperature, the deposited product is isolated by filtering off with suction, washed with water and dried under reduced pressure at 50° C. 32.5 g (0.1 mol=91% of theory) of a solid of m.p.: 257°-258° C. are obtained. A combustion analysis gave an iodine content of 38.5% (theory 39.3%).

후처리

  1. stirringit is stirred at 5° C. for 30 min
  2. customnitrogen being formed
  3. temperatureAfter cooling to room temperature
  4. customthe deposited product is isolated
  5. filtrationby filtering off with suction
  6. washwashed with water
  7. customdried under reduced pressure at 50° C
  8. custom32.5 g (0.1 mol=91% of theory) of a solid of m.p.: 257°-258° C. are obtained

출처 및 근거

ORD 기록
ord-7fc91a129aeb4cb09cfa6ba7c7b4f71f
출처 데이터셋
uspto-grants-1999_01
특허 번호
US05863864

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