Water → HCID 59310059、化合物

HRID 1512973ノート

反応式

HRID 1512973 の反応式
O.S(=O)(=O)(O)O.[Cl:7][C:8]1[CH:14]=[CH:13][C:12]([SH:15])=[CH:11][C:9]=1[NH2:10].[C:16]1([C:22](O)([CH3:24])[CH3:23])[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1>O1CCCC1>[Cl:7][C:8]1[CH:14]=[CH:13][C:12]([S:15][C:22]([CH3:24])([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH3:23])=[CH:11][C:9]=1[NH2:10]

参加物

6

反応物 4

HCID 962WaterHCID 1118Sulfuric AcidHCID 120532-Phenyl-2-propanolHCID 6406993-amino-4-chlorobenzenethiol

生成物 1

HCID 59310059HCID 59310059、化合物収率 58.4%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a mixture of water (10 mL) and concentrated sulfuric acid (10 mL) was added 2-chloro-5-mercaptoaniline (1.6 g) at room temperature, and the mixture was stirred for 15 minutes. To the mixture was added a solution of 2-phenyl-2-propanol (1.36 g) in tetrahydrofuran (10 mL) in a dropwise manner, and the mixture was stirred at room temperature for 30 minutes. The reaction mixture was poured into ice water, and the resulting mixture was extracted with ethyl acetate. The extract was washed with water, a saturated aqueous sodium hydrogen carbonate solution and brine successively, and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure, and the residue was purified by column chromatography on silica gel (eluent: n-hexane−n-hexane/ethyl acetate=4/1) to give the title compound (1.62 g).

後処理

  1. stirringthe mixture was stirred at room temperature for 30 minutes
  2. extractionthe resulting mixture was extracted with ethyl acetate
  3. washThe extract was washed with water
  4. dry with materiala saturated aqueous sodium hydrogen carbonate solution and brine successively, and dried over anhydrous magnesium sulfate
  5. customThe solvent was removed under reduced pressure
  6. customthe residue was purified by column chromatography on silica gel (eluent: n-hexane−n-hexane/ethyl acetate=4/1)

出典と根拠

ORDレコード
ord-b8e210f98fd24b6fbd66f5d3e45f1c01
出典データセット
uspto-grants-2012_07
特許番号
US08217069B2

反応ノート

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