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Benzoyl chloride → 5-Amidino-2-benzoyloxybenzenesulfonic acid

HRID 1589493
ノート
印刷プレビュー

反応式

HRID 1589493 の反応式
[C:1]([C:4]1[CH:5]=[CH:6][C:7]([OH:14])=[C:8]([S:10]([OH:13])(=[O:12])=[O:11])[CH:9]=1)(=[NH:3])[NH2:2].[C:15](Cl)(=[O:22])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1>N1C=CC=CC=1>[C:1]([C:4]1[CH:5]=[CH:6][C:7]([O:14][C:15](=[O:22])[C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)=[C:8]([S:10]([OH:13])(=[O:11])=[O:12])[CH:9]=1)(=[NH:2])[NH2:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 7412Benzoyl chlorideHCID 1355987485-Amidino-2-hydroxybenzenesulfonic acid

生成物 1

HCID 131784555-Amidino-2-benzoyloxybenzenesulfonic acid

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To 30 ml of dried pyridine, was added 3.0 g of 5-amidino-2-hydroxybenzenesulfonic acid. To the mixture, while being cooled in ice, was slowly added dropwise 2.0 g of benzoyl chloride. After the addition, the mixture was stirred overnight at room temperature. The insolubles deposited from the reaction mixture were separated by filtration, washed with pyridine, then with water, finally with acetone, and suspended in methanol. The insolubles were removed by filtration, and ethyl ether was added to the filtrate to precipitate a colorless solid. The solid was collected by filtration and recrystallized from a methanol-ethyl ether mixture to obtain 5-amidino-2-benzoyloxybenzenesulfonic acid in colorless solid form.

後処理

  1. temperatureTo the mixture, while being cooled in ice
  2. additionAfter the addition
  3. customwere separated by filtration
  4. washwashed with pyridine
  5. customThe insolubles were removed by filtration, and ethyl ether
  6. additionwas added to the filtrate
  7. customto precipitate a colorless solid
  8. filtrationThe solid was collected by filtration
  9. customrecrystallized from a methanol-ethyl ether mixture

出典と根拠

ORDレコード
ord-45f39bccb09646ec89d52299996826ba
出典データセット
uspto-grants-1986_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04570006

反応ノート

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