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Iodoethane → HCID 68538880、化合物

HRID 852542
ノート
印刷プレビュー

反応式

HRID 852542 の反応式
C([O-])([O-])=O.[K+].[K+].I[CH2:8][CH3:9].[CH3:10][O:11][C:12](=[O:24])[C:13]1[CH:22]=[C:21]([OH:23])[CH:20]=[C:15]([C:16]([O:18][CH3:19])=[O:17])[CH:14]=1>CC(C)=O>[CH3:19][O:18][C:16](=[O:17])[C:15]1[CH:20]=[C:21]([O:23][CH2:8][CH3:9])[CH:22]=[C:13]([C:12]([O:11][CH3:10])=[O:24])[CH:14]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 830651,3-Benzenedicarboxylic acid, 5-hydroxy-, 1,3-dimethyl ester

生成物 1

HCID 68538880HCID 68538880、化合物収率 96.5%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

K2CO3 (31.6 g, 223 mmol, 2.23 equiv) and iodoethane (17.8 ml, 230 mmol, 2.3 equiv) were added to a solution of 5-hydroxy-isophthalic acid dimethyl ester (D42) (21 g, 100 mmol, 1 equiv) in acetone (500 ml) at room temperature. The resulting solution was refluxed for 16 h, then cooled to room temperature and concentrated in vacuo. The residue was partitioned between H2O and AcOEt. The aqueous phase was extracted with AcOEt and the combined organic layers were washed with 2N aqueous NaOH solution and brine, dried over MgSO4 and concentrated in vacuo to give 5-ethoxy-isophthalic acid dimethyl ester (D43) (23 g, 96%) as a white solid. RT=3.13 min

後処理

  1. temperatureThe resulting solution was refluxed for 16 h
  2. concentrationconcentrated in vacuo
  3. customThe residue was partitioned between H2O and AcOEt
  4. extractionThe aqueous phase was extracted with AcOEt
  5. washthe combined organic layers were washed with 2N aqueous NaOH solution and brine
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-f3f407b290094123a34e68ec9fe9ea4a
出典データセット
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07253198B2

反応ノート

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