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

HRID 1776376노트

반응식

HRID 1776376 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 702EthanolHCID 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) 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-cb42669ed9bb44a9b2bf66c688100d26
출처 데이터셋
uspto-grants-2016_02
특허 번호
US09265767B2

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