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Dimethylformamide → HCID 59496797、化合物

HRID 416985
ノート
印刷プレビュー

反応式

HRID 416985 の反応式
[CH2:1]([O:3][C:4](=[O:37])[CH2:5][CH2:6][CH2:7][O:8][C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][O:21][C:22]2[CH:27]=[C:26]([OH:28])[CH:25]=[C:24]([Br:29])[CH:23]=2)[C:10]=1[CH2:30][CH2:31][C:32]([O:34][CH2:35][CH3:36])=[O:33])[CH3:2].C(=O)([O-])[O-].[K+].[K+].CN(C)C=O.I[CH2:50][CH3:51]>O.CC(C)=O>[CH2:1]([O:3][C:4](=[O:37])[CH2:5][CH2:6][CH2:7][O:8][C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][O:21][C:22]2[CH:27]=[C:26]([O:28][CH2:50][CH3:51])[CH:25]=[C:24]([Br:29])[CH:23]=2)[C:10]=1[CH2:30][CH2:31][C:32]([O:34][CH2:35][CH3:36])=[O:33])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 6228DimethylformamideHCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 59496799HCID 59496799、化合物

生成物 1

HCID 59496797HCID 59496797、化合物収率 98%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒
HCID 962
Water
溶媒

実験手順

To a mixture of 4-[3-[6-(3-bromo-5-hydroxy-phenoxy)-hexyl]-2-(2-ethoxycarbonyl-ethyl)-phenoxy]-butyric acid ethyl ester (163 mg, 0.28 mmol) and potassium carbonate (117 mg, 0.84 mmol) were added dimethylformamide (4 mL), acetone (8 mL), and iodoethane (219 mg, 1.4 mmol) at room temperature. The resulting suspension was heated to reflux for 2 days. Then, the reaction mixture was cooled to room temperature and diluted with water (20 mL). The organic compound was extracted into ethyl acetate (2×25 mL) and the combined organic extracts were washed with water (50 mL) and brine solution (50 mL). The organic layers were dried over anhydrous magnesium sulfate and filtration of the drying agent and concentration of the solvent gave the crude product which was purified by using an ISCO 40 g column, eluting with 0-30% ethyl acetate in hexanes to afford 4-[3-[6-(3-bromo-5-ethoxy-phenoxy)-hexyl]-2-(2-ethoxycarbonyl-ethyl)-phenoxy]-butyric acid ethyl ester (166 mg, 98%) as a colorless oil: ES(+)-HRMS m/e calcd for C31H43BrO7 (M+H)+ 607.2265. found 607.2270.

後処理

  1. temperatureThe resulting suspension was heated
  2. temperatureto reflux for 2 days
  3. extractionThe organic compound was extracted into ethyl acetate (2×25 mL)
  4. washthe combined organic extracts were washed with water (50 mL) and brine solution (50 mL)
  5. dry with materialThe organic layers were dried over anhydrous magnesium sulfate and filtration of the drying agent and concentration of the solvent
  6. customgave the crude product which
  7. customwas purified
  8. washeluting with 0-30% ethyl acetate in hexanes

出典と根拠

ORDレコード
ord-365f267334e944c0913d7c88363d0e9c
出典データセット
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08088936B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート