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

HRID 1258351노트

반응식

HRID 1258351 반응식
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

참가 물질

4

반응물 3

HCID 702Ethanol2회HCID 8021DiethylamineHCID 59354791HCID 59354791, 화합물

생성물 1

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

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-813ef0785df24ad08bcdb0f076c5d9c6
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08466148B2

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