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Ethyl Acetate → 2-Amino-6-chlorobenzenethiol hydrogen chloride, 95%

HRID 1370501
ノート
印刷プレビュー

反応式

HRID 1370501 の反応式
C([S:8][C:9]1[C:14]([Cl:15])=[CH:13][CH:12]=[CH:11][C:10]=1[NH2:16])C1C=CC=CC=1.[Al+3].[Cl-].[Cl-].[Cl-].CCOC(C)=O>C1C=CC=CC=1>[ClH:15].[NH2:16][C:10]1[CH:11]=[CH:12][CH:13]=[C:14]([Cl:15])[C:9]=1[SH:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8857Ethyl AcetateHCID 6451240Aluminum(III) ChlorideHCID 13782476HCID 13782476、化合物

生成物 1

HCID 185116192-Amino-6-chlorobenzenethiol hydrogen chloride, 95%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

To a solution of 2-benzylsulfanyl-3-chloro-phenylamine (204) in 140 mL of benzene at 0° C. was added AlCl3 (Aldrich, 23.8 g, 179 mmol) in portion. The mixture turned to purple. After stirred at ambient temperature overnight, the mixture was poured to ice and EtOAc and stirred for 20 min. The mixture was extracted 3× with EtOAc (500 mL). The organic layers were washed twice with a brine solution (400 mL), dried over Na2SO4, and concentrated under vacuum. The crude product was treated with 145 mL of 1N HCl in ether. The product (13.6 g) was collected by filtration and washed with hexanes.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. stirringstirred for 20 min
  2. extractionThe mixture was extracted 3× with EtOAc (500 mL)
  3. washThe organic layers were washed twice with a brine solution (400 mL)
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated under vacuum
  6. additionThe crude product was treated with 145 mL of 1N HCl in ether
  7. filtrationThe product (13.6 g) was collected by filtration
  8. washwashed with hexanes

出典と根拠

ORDレコード
ord-a31239af8e1a403da743eca655007945
出典データセット
uspto-grants-2003_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06583157B2

反応ノート

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