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Formaldehyde → HCID 11776435、化合物

HRID 1720672
ノート
印刷プレビュー

反応式

HRID 1720672 の反応式
[Cl-].[Li+].C(OP([CH:11]([CH2:17][C:18]1[C:27]2[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=2)[CH:21]=[CH:20][CH:19]=1)[C:12]([O:14][CH2:15][CH3:16])=[O:13])(OCC)=O)C.[CH2:28]1CCN2C(=NCCC2)CC1.C=O>C1COCC1>[C:18]1([CH2:17][C:11](=[CH2:28])[C:12]([O:14][CH2:15][CH3:16])=[O:13])[C:27]2[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=2)[CH:21]=[CH:20][CH:19]=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 712FormaldehydeHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 270093Ethyl 2-(diethoxyphosphoryl)-3-(naphthalen-1-yl)propanoateHCID 433294Lithium Chloride

生成物 1

HCID 11776435HCID 11776435、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒3 回

実験手順

1.92 g of lithium chloride was suspended-in 50 ml of dry THF, and 15 g of ethyl 2-diethylphosphono-3-(1-naphthyl)propionate was dropwise added thereto. Then, 16 ml of a 50% dry THF solution of DBU was dropwise added thereto, and 2.01 g of paraformaldehyde suspended in dry THF was added thereto. The mixture was stirred at room temperature for 3 hours, and the insolubles were removed by filtration and washed with a small amount of diethyl ether. The washing solution and and the filtrate were put together, and the solvent was distilled off. The resulting syrup was dissolved in 180 ml of diethyl ether. The diethyl ether layer was washed sequentially with a 10% citric acid aqueous solution, with water and with a saturated sodium chloride aqueous solution and dried over anhydride sodium sulfate. The solvent was distilled off, and the syrup thereby obtained was purified by silica gel column chromatography (n-hexane/diethyl ether=20/1) to obtain 6.48 g of ethyl 2-(1-naphthyl)methyl-2-propenoate as colorless oily substance.

後処理

  1. additionwas added
  2. customthe insolubles were removed by filtration
  3. washwashed with a small amount of diethyl ether
  4. distillationthe solvent was distilled off
  5. dissolutionThe resulting syrup was dissolved in 180 ml of diethyl ether
  6. washThe diethyl ether layer was washed sequentially with a 10% citric acid aqueous solution, with water and with a saturated sodium chloride aqueous solution
  7. dry with materialdried over anhydride sodium sulfate
  8. distillationThe solvent was distilled off
  9. customthe syrup thereby obtained
  10. customwas purified by silica gel column chromatography (n-hexane/diethyl ether=20/1)

出典と根拠

ORDレコード
ord-598ffbb2a52d42c881e6a0ee975d2a3b
出典データセット
uspto-grants-1996_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05506356

反応ノート

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