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

HRID 436548

反応式

HRID 436548 の反応式
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]

参加物

8

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 3776Isopropanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3e871e83a4f9492bbd2264290214c3df
出典データセット
uspto-grants-1977_02
特許番号
US04009205

関連ノート

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