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

HRID 1448083ノート

反応式

HRID 1448083 の反応式
[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]

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6dfc33a7e6d34f0db5d588030af4a4f3
出典データセット
uspto-grants-1979_12
特許番号
US04179514

反応ノート

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