Sodium Hydroxide → 4-Amino-1-naphthaldehyde

HRID 1166788

반응식

HRID 1166788 반응식
[S].[N+:2]([C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[C:8]([CH3:15])=[CH:7][CH:6]=1)([O-])=O.[OH-:16].[Na+]>C(O)C.C(OCC)(=O)C>[NH2:2][C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[C:8]([CH:15]=[O:16])=[CH:7][CH:6]=1

참가 물질

6

반응물 3

HCID 14798Sodium HydroxideHCID 701554-Methyl-1-nitronaphthaleneHCID 5362487Sulfur

생성물 1

HCID 229991604-Amino-1-naphthaldehyde

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8857Ethyl Acetate용매

실험 절차

To a stirring boiling solution of sulfur (3.7 g) in 12% aqueous NaOH (50 mL) was added a solution of 4-nitro-1-methylnaphthalene (8 g) in ethanol (50 mL). After refluxing the solution for one hour, the reaction was diluted with 500 mL of ethyl acetate and washed with water and brine, dried over MgSO4, and concentrated. The product was purified via silica gel column chromatography using ethyl acetate:hexane (5:95 to 10:90). The product (2.54 g, 34%) was stored at −78° C.

후처리

  1. temperatureAfter refluxing the solution for one hour
  2. washwashed with water and brine
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated
  5. customThe product was purified via silica gel column chromatography
  6. customwas stored at −78° C.

출처 및 근거

ORD 기록
ord-8d668a3fd8f045c186ceef8d2ef27b55
출처 데이터셋
uspto-grants-2003_09
특허 번호
US06613942B1

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