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CID 406 → Methyl [3-[2-(4,5-diphenyl-2-oxazolyl)ethenyl]phenoxy]acetate

HRID 257626
ノート
印刷プレビュー

反応式

HRID 257626 の反応式
[Na].[C:2]1([C:8]2[N:9]=[C:10]([CH2:19]P(=O)(OC)OC)[O:11][C:12]=2[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH:26]([C:28]1[CH:29]=[C:30]([CH:37]=[CH:38][CH:39]=1)[O:31][CH2:32][C:33]([O:35][CH3:36])=[O:34])=O.P(=O)([O-])[O-]>CO>[C:2]1([C:8]2[N:9]=[C:10]([CH:19]=[CH:26][C:28]3[CH:29]=[C:30]([CH:37]=[CH:38][CH:39]=3)[O:31][CH2:32][C:33]([O:35][CH3:36])=[O:34])[O:11][C:12]=2[C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=2)[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=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 406CID 406HCID 1494380Methyl 2-(3-formylphenoxy)acetateHCID 5360545SodiumHCID 54445617Dimethyl [(4,5-diphenyl-2-oxazolyl)methyl]phosphonate

生成物 1

HCID 53907733Methyl [3-[2-(4,5-diphenyl-2-oxazolyl)ethenyl]phenoxy]acetate

試薬・触媒・溶媒 1

HCID 887Methanol
溶媒

実験手順

Sodium metal (260 mg, 11 mg atom) was dissolved in methanol (50 mL) and dimethyl [(4,5-diphenyl-2-oxazolyl)methyl]phosphonate (3.89 g, 11 mmol) added followed by methyl (3-formylphenoxy)acetate (2 g, 10 mmol). The mixture was stirred at room temperature for 20 minutes before being concentrated and diluted with 2N HCl solution. The mixture was extracted with CH2Cl2, the organic phase dried over sodium sulfate and the solvent evaported to leave a yellow oil. This was combined with the crude material from a reaction performed on 2 g of the phosphonate and 985 mg of aldehyde and chromatographed on a column of silica gel. Elution with a mixture of hexanes and diethyl ether (3:2) furnished methyl [3-[2-(4,5-diphenyl-2-oxazolyl)ethenyl]phenoxy]acetate as the diethyl ether solvate (2.92 g, 46%) after recrystallization from diethyl ether, m.p. 79°-82° C.

後処理

  1. concentrationbefore being concentrated
  2. additiondiluted with 2N HCl solution
  3. extractionThe mixture was extracted with CH2Cl2
  4. dry with materialthe organic phase dried over sodium sulfate
  5. customto leave a yellow oil
  6. customchromatographed on a column of silica gel
  7. washElution
  8. additionwith a mixture of hexanes and diethyl ether (3:2)

出典と根拠

ORDレコード
ord-b6b259a1f7cc441f9591b6800a523a2e
出典データセット
uspto-grants-1993_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05262540

反応ノート

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