Sulfuric Acid → 4-Amino-3-methyl-N-ethyl-N-(beta-(methanesulfonamido)ethyl)aniline

HRID 436548

반응식

HRID 436548 반응식
C1(C)C=CC(S([NH:10][C:11]2[CH:19]=[CH:18][C:14]([NH:15][CH2:16][CH3:17])=[CH:13][C:12]=2[CH3:20])(=O)=O)=CC=1.[CH3:22][S:23]([NH:26][CH2:27][CH2:28]Cl)(=[O:25])=[O:24].C(=O)([O-])O.[Na+].S(=O)(=O)(O)O>C(O)(C)C.CO.O>[NH2:10][C:11]1[CH:19]=[CH:18][C:14]([N:15]([CH2:28][CH2:27][NH:26][S:23]([CH3:22])(=[O:25])=[O:24])[CH2:16][CH3:17])=[CH:13][C:12]=1[CH3:20]

참가 물질

8

반응물 4

HCID 1118Sulfuric AcidHCID 89092N-(2-Chloroethyl)methanesulphonamideHCID 516892Sodium BicarbonateHCID 214528354-(N-p-Toluenesulfonyl)amino-3-methyl-N-ethylaniline

생성물 1

HCID 666934-Amino-3-methyl-N-ethyl-N-(beta-(methanesulfonamido)ethyl)aniline

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 3776Isopropanol용매

실험 절차

A mixture of 7g of 4-(N-p-toluenesulfonyl)amino-3-methyl-N-ethylaniline, 4g of β-methanesulfonamidoethyl chloride, 2.1g of sodium hydrogen carbonate, 16g of water and 30ml of methanol were refluxed for 5 hours, and then 16g of sulfuric acid were added thereto and the entire reaction system was again refluxed. Next, the reaction solution was condensed to half the original volume and 300ml of isopropyl alcohol were added thereto to separate crystals. The crystals were filtered out and dried to obtain 1.5g of 4-amino-3-methyl-N-(β-methanesulfonamidoethyl)-N-ethylaniline. sesquisulfate. H2O.

후처리

  1. temperaturewere refluxed for 5 hours
  2. temperaturethe entire reaction system was again refluxed
  3. additionwere added
  4. customto separate crystals
  5. filtrationThe crystals were filtered out
  6. customdried

출처 및 근거

ORD 기록
ord-3e871e83a4f9492bbd2264290214c3df
출처 데이터셋
uspto-grants-1977_02
특허 번호
US04009205

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