Ethyl bromoacetate → HCID 11287642、化合物

HRID 2056265ノート

反応式

HRID 2056265 の反応式
[OH:1][C:2]1[CH:6]=[C:5]([C:7]([O:9][CH3:10])=[O:8])[O:4][N:3]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:18][C:19]([O:21][CH2:22][CH3:23])=[O:20]>CC(C)=O>[CH3:10][O:9][C:7]([C:5]1[O:4][N:3]=[C:2]([O:1][CH2:18][C:19]([O:21][CH2:22][CH3:23])=[O:20])[CH:6]=1)=[O:8]

参加物

5

反応物 3

HCID 7748Ethyl bromoacetateHCID 11430Potassium CarbonateHCID 178498603HCID 178498603、化合物

生成物 1

HCID 11287642HCID 11287642、化合物収率 81%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a solution of methyl 3-hydroxy-isoxazole-5-carboxylate (7.14 mmol) in acetone (30 mL), was added potassium carbonate (1.2 g, 8.6 mmol) and ethyl bromoacetate (8.6 mmol). The reaction mixture was heated at reflux for 2 h, monitoring by TLC. At completion, acetone was removed in vacuo and the residue partitioned between water and ethyl acetate (50 mL). The organic layer was dried (MgSO4), filtered, and evaporated to afford the desired intermediate.

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux for 2 h
  3. customAt completion, acetone was removed in vacuo
  4. customthe residue partitioned between water and ethyl acetate (50 mL)
  5. dry with materialThe organic layer was dried (MgSO4)
  6. filtrationfiltered
  7. customevaporated

出典と根拠

ORDレコード
ord-82811266ae484c7f923d9f075aa82098
出典データセット
uspto-grants-2008_02
特許番号
US07335655B2

反応ノート

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