Ethyl bromoacetate → Ethyl 2-(4-methoxyphenyl)sulfanylacetate

HRID 2422213

反応式

HRID 2422213 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([SH:9])=[CH:5][CH:4]=1.C(N(CC)CC)C.O1CCCC1.Br[CH2:23][C:24]([O:26][CH2:27][CH3:28])=[O:25]>C(O)C>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([S:9][CH2:23][C:24]([O:26][CH2:27][CH3:28])=[O:25])=[CH:5][CH:4]=1

参加物

6

反応物 4

HCID 7748Ethyl bromoacetateHCID 8028TetrahydrofuranHCID 8471TriethylamineHCID 127654-Methoxybenzenethiol

生成物 1

HCID 1482371Ethyl 2-(4-methoxyphenyl)sulfanylacetate収率 92%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To an ice-cooled mixture of 4-methoxythiophenol (15 g, 0.11 mol), triethylamine (28 mL, 0.20 mol) and tetrahydrofuran (150 mL) was added ethyl bromoacetate (21 g, 0.13 mol), and the mixture was stirred overnight at room temperature. Ethanol (10 mL) was added, the solvent was evaporated under reduced pressure, and the residue was partitioned between ethyl acetate and water. The organic layer was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=10:1) to give title compound (22 g, yield 92%). oil.

後処理

  1. customthe solvent was evaporated under reduced pressure
  2. customthe residue was partitioned between ethyl acetate and water
  3. concentrationThe organic layer was concentrated under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=10:1)

出典と根拠

ORDレコード
ord-42d83b6449764e33977a6b0946c3f50d
出典データセット
uspto-grants-2011_06
特許番号
US07960369B2

関連ノート

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