4-Amino-1-naphthalenesulfonic acid → 4-Methanesulfonamido-1-naphthalene sulfonic acid pyridinium salt

HRID 366978

反応式

HRID 366978 の反応式
[NH2:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([S:12]([OH:15])(=[O:14])=[O:13])=[CH:4][CH:3]=1.[CH3:16][S:17](Cl)(=[O:19])=[O:18]>N1C=CC=CC=1>[NH+:1]1[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1.[CH3:16][S:17]([NH:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([S:12]([O-:15])(=[O:13])=[O:14])=[CH:4][CH:3]=1)(=[O:19])=[O:18]

参加物

4

反応物 2

HCID 67904-Amino-1-naphthalenesulfonic acidHCID 31297Methanesulfonyl chloride

生成物 1

HCID 1317221234-Methanesulfonamido-1-naphthalene sulfonic acid pyridinium salt収率 123.7%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A suspension of 4-amino-1-naphthalene sulfonic acid (200 g, 0.897 mole) in 800 ml of pyridine was stirred mechanically while methanesulfonyl chloride (70 ml, 0.9 mole) was added slowly over about 10 min. The reaction warmed to about 60° as the solid dissolved and then slowly cooled to room temperature. The mixture was stirred overnight while a solid precipitated. After filtering and washing with 500 ml of ether, the solid was dried under a nitrogen stream to afford 211 g (62%) of 4-methanesulfonamido-1-naphthalene sulfonic acid pyridinium salt.

後処理

  1. additionwas added slowly over about 10 min
  2. temperatureThe reaction warmed to about 60° as the solid
  3. dissolutiondissolved
  4. customprecipitated
  5. filtrationAfter filtering
  6. washwashing with 500 ml of ether
  7. customthe solid was dried under a nitrogen stream

出典と根拠

ORDレコード
ord-ae77841f510f4d268915f374c19db12b
出典データセット
uspto-grants-2000_10
特許番号
US06132944

関連ノート

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