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Water → Tert-butyl 2-(3-pyridyloxy)acetate

HRID 1007172
ノート
印刷プレビュー

反応式

HRID 1007172 の反応式
[H-].[Na+].[OH:3][C:4]1[CH:5]=[N:6][CH:7]=[CH:8][CH:9]=1.Br[CH2:11][C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13].O>CN(C=O)C>[N:6]1[CH:7]=[CH:8][CH:9]=[C:4]([O:3][CH2:11][C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH:5]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 79713-HydroxypyridineHCID 24758Sodium hydrideHCID 79177tert-Butyl bromoacetate

生成物 1

HCID 22668053Tert-butyl 2-(3-pyridyloxy)acetate収率 32.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

To a suspension of 0.22 g of sodium hydride (60% oil dispersion, 5.5 mmol) in 2 mL of DMF was added dropwise a solution of 0.48 g of 3-hydroxypyridine (5.0 mmol) in 2 mL of DMF at room temperature, and the mixture was stirred for an hour. The resulting brown solution was ice-cooled, 0.81 mL of tert-butyl bromoacetate (5.5 mmol) was added, and the mixture was stirred under ice-cooling for an hour followed by stirring at room temperature for 2 hours. After addition of water, the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried and evaporated. The residue was purified by column chromatography on silica gel (eluent: chloroform:ethyl acetate=5:1), to give 0.34 g of tert-butyl 3-pyridyloxyacetate (Yield: 32.5%) as a clear oil.

後処理

  1. temperaturecooled
  2. stirringthe mixture was stirred under ice-
  3. temperaturecooling for an hour
  4. stirringby stirring at room temperature for 2 hours
  5. extractionthe mixture was extracted with ethyl acetate
  6. washThe organic layer was washed with saturated brine
  7. customdried
  8. customevaporated
  9. customThe residue was purified by column chromatography on silica gel (eluent: chloroform:ethyl acetate=5:1)

出典と根拠

ORDレコード
ord-cd238d212d81494dbda0f998d1b0dd42
出典データセット
uspto-grants-2004_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06794392B1

反応ノート

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