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

HRID 1602486
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HRID 1602486 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 196113194-[3-(4-Chlorophenylsulfonyl)propyl]-2-nitrophenolHCID 178418361HCID 178418361, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매
HCID 31275
1,4-Dioxane
용매
2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7dce7a6038b54962bb0b11c56d208334
출처 데이터셋
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05981559

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