1-Naphthol → 1-[N-methyl-N-(2,4-dimethyl-3-oxo-2-pentanesulfenyl)carbamoyloxy]-napthalene

HRID 1448083노트

반응식

HRID 1448083 반응식
[CH3:1][N:2]([S:6][C:7]([CH3:14])([C:9](=[O:13])[CH:10]([CH3:12])[CH3:11])[CH3:8])[C:3](Cl)=[O:4].[C:15]1([OH:25])[C:24]2[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=2)[CH:18]=[CH:17][CH:16]=1.C(N(CC)CC)C.C(OCC)(=O)C>O1CCOCC1.O>[CH3:1][N:2]([S:6][C:7]([CH3:14])([C:9](=[O:13])[CH:10]([CH3:12])[CH3:11])[CH3:8])[C:3]([O:25][C:15]1[C:24]2[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=2)[CH:18]=[CH:17][CH:16]=1)=[O:4]

참가 물질

7

반응물 4

HCID 70051-NaphtholHCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 54024146N-methyl-N-(2,4-dimethyl-3-oxo-2-pentanesulfenyl)carbamoyl chloride

생성물 1

HCID 540653211-[N-methyl-N-(2,4-dimethyl-3-oxo-2-pentanesulfenyl)carbamoyloxy]-napthalene수율 64.7%

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매

실험 절차

To a solution of 10.0 g (0.042 m) of N-methyl-N-(2,4-dimethyl-3-oxo-2-pentanesulfenyl)carbamoyl chloride and 6.06 g (0.042 m) of 1-naphthol in 75 ml of dioxane was added 4.26 g (0.042 m) of triethylamine. After stirring at room temperature for 17 hours the reaction mixture was diluted with 500 ml of cold water and the product taken into ethyl acetate. The organic phase was washed in turn with 1.0 percent sodium hydroxide and water and then dried over magnesium sulfate. On removal of the solvent it yielded 9.4 g of a residual oil.

후처리

  1. washThe organic phase was washed in turn with 1.0 percent sodium hydroxide and water
  2. dry with materialdried over magnesium sulfate
  3. customOn removal of the solvent it

출처 및 근거

ORD 기록
ord-6dfc33a7e6d34f0db5d588030af4a4f3
출처 데이터셋
uspto-grants-1979_12
특허 번호
US04179514

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