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Hydrochloric Acid → 2-Amino-4-[3-(4-chlorophenylsulfonyl)propyl]phenol hydrochloride

HRID 1602486
ノート
印刷プレビュー

反応式

HRID 1602486 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([CH2:11][CH2:12][CH2:13][C:14]2[CH:19]=[CH:18][C:17]([OH:20])=[C:16]([N+:21]([O-])=O)[CH:15]=2)(=[O:10])=[O:9])=[CH:4][CH:3]=1.Cl.[H][H]>O1CCOCC1.[C].[Pd]>[ClH:1].[NH2:21][C:16]1[CH:15]=[C:14]([CH2:13][CH2:12][CH2:11][S:8]([C:5]2[CH:6]=[CH:7][C:2]([Cl:1])=[CH:3][CH:4]=2)(=[O:10])=[O:9])[CH:19]=[CH:18][C:17]=1[OH:20]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 196113194-[3-(4-Chlorophenylsulfonyl)propyl]-2-nitrophenolHCID 178418361HCID 178418361、化合物

生成物 1

HCID 196115102-Amino-4-[3-(4-chlorophenylsulfonyl)propyl]phenol hydrochloride収率 190.7%

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒
HCID 31275
1,4-Dioxane
溶媒
2 回

実験手順

4-[3-(4-Chlorophenylsulfonyl)propyl]-2-nitrophenol (10.00 g, 28.11 mmol) was dissolved in 1,4-dioxane (100 ml), 4 N hydrochloric acid solution in 1,4-dioxane (8.43 ml, 33.73 mmol) and 10% palladium-carbon (1.0 g) were added, and the mixture was stirred for 4 hours in an atmosphere of hydrogen gas under 1 atmospheric pressure. The crystals precipitated in the reaction solution were dissolved by adding methanol, the reaction mixture was filtered, and then the resulting filtrate was concentrated under reduced pressure. By crystallizing the resulting residue from acetonitrile-ether, 2-amino-4-[3-(4-chlorophenylsulfonyl)propyl]phenol hydrochloride (9.71 g, 95%) was obtained.

後処理

  1. customThe crystals precipitated in the reaction solution
  2. dissolutionwere dissolved
  3. additionby adding methanol
  4. filtrationthe reaction mixture was filtered
  5. concentrationthe resulting filtrate was concentrated under reduced pressure
  6. customBy crystallizing the resulting residue from acetonitrile-ether

出典と根拠

ORDレコード
ord-7dce7a6038b54962bb0b11c56d208334
出典データセット
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05981559

反応ノート

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