Hydrochloric Acid → 3-(N-methylamino)aniline-4-sulfonic acid

HRID 1197210

반응식

HRID 1197210 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([OH:11])(=[O:10])=[O:9])=[C:4]([NH2:12])[CH:3]=1.[C:13](OC(=O)C)(=O)C.[OH-].[Na+].S(OC)(OC)(=O)=O.Cl.[Cl-].[Na+]>O.C(O)=O>[CH3:13][NH:12][C:4]1[CH:3]=[C:2]([CH:7]=[CH:6][C:5]=1[S:8]([OH:11])(=[O:9])=[O:10])[NH2:1]

참가 물질

9

반응물 6

HCID 313Hydrochloric AcidHCID 5234Sodium ChlorideHCID 6497Dimethyl SulfateHCID 7918Acetic AnhydrideHCID 14798Sodium Hydroxide3회HCID 666232,4-Diaminobenzenesulfonic acid

생성물 1

HCID 109655703-(N-methylamino)aniline-4-sulfonic acid

시약·촉매·용매 2

HCID 284Formic Acid용매HCID 962Water용매

반응 조건

온도
20 °C

실험 절차

94 g of 1,3-diaminobenzene-4-sulfonic acid in 430 ml of water and 70 g of formic acid were boiled for 3 hours under reflux. The mixture was cooled to 20° C., and the resulting 3-(N-formylamino)aniline-4-sulfonic acid was filtered off in vacuo and stirred in 500 g of water with the addition of caustic soda solution to give a pH of 6.5. 70 g of acetic anhydride were then added and the pH was kept between 5.0 and 6.5 by the addition of caustic soda solution. After 30 minutes, the pH was adjusted to 12.5 with caustic soda solution, and 75 g of dimethyl sulfate were added dropwise. After 30 minutes, the pH was adjusted to -0.5 with hydrochloric acid, and the mixture was boiled under reflux for 3 hours. After cooling, the mixture was adjusted to pH 1.0 with caustic soda solution and salted out with 150 g of sodium chloride. The precipitated 3-(N-methylamino)aniline- 4-sulfonic acid was isolated by filtration in vacuo.

후처리

  1. temperatureunder reflux
  2. filtrationthe resulting 3-(N-formylamino)aniline-4-sulfonic acid was filtered off in vacuo
  3. customto give a pH of 6.5
  4. additionwere added dropwise
  5. waitAfter 30 minutes
  6. temperatureunder reflux for 3 hours
  7. temperatureAfter cooling

출처 및 근거

ORD 기록
ord-d46403aea0164f58b488fbb708d4e92a
출처 데이터셋
uspto-grants-1992_05
특허 번호
US05117050

연결된 노트

불러오는 중…