Ethanol → 2-(Pyridin-4-yl)-1-oxaspiro[4.4]non-2-en-4-one

HRID 1258351ノート

反応式

HRID 1258351 の反応式
O[C:2]1([C:7]#[C:8][C:9]([C:11]2[CH:16]=[CH:15][N:14]=[CH:13][CH:12]=2)=[O:10])[CH2:6][CH2:5][CH2:4][CH2:3]1.C(NCC)C.C([OH:24])C>>[N:14]1[CH:15]=[CH:16][C:11]([C:9]2[O:10][C:2]3([CH2:6][CH2:5][CH2:4][CH2:3]3)[C:7](=[O:24])[CH:8]=2)=[CH:12][CH:13]=1

参加物

4

反応物 3

HCID 702Ethanol2 回HCID 8021DiethylamineHCID 59354791HCID 59354791、化合物

生成物 1

HCID 593547772-(Pyridin-4-yl)-1-oxaspiro[4.4]non-2-en-4-one

実験手順

To a stirred solution of 3-(1-hydroxycyclopentyl)-1-(pyridin-4-yl) prop-2-yn-1-one (0.42 g, 1.95 mmol) in ethanol (10 mL) was added diethyl amine (0.21 g, 2.9 mmol) in EtOH (1 mL) dropwise at RT and the reaction mixture was stirred for additional 1 h. Then the EtOH was removed, diluted with EtOAc (20 mL), washed with water (10 mL), brine (10 mL), dried over Na2SO4, filtered and concentrated in vacuo to afford 2-(pyridin-4-yl)-1-oxaspiro[4.4]non-2-en-4-one (0.4 g) as an oil.

後処理

  1. customThen the EtOH was removed
  2. additiondiluted with EtOAc (20 mL)
  3. washwashed with water (10 mL), brine (10 mL)
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-813ef0785df24ad08bcdb0f076c5d9c6
出典データセット
uspto-grants-2013_06
特許番号
US08466148B2

反応ノート

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