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3,4-dihydro-2H-pyran → HCID 117874872、化合物

HRID 517369
ノート
印刷プレビュー

反応式

HRID 517369 の反応式
[F:1][C:2]([F:26])([F:25])[C:3]1[CH:4]=[C:5]([CH:22]=[CH:23][CH:24]=1)[O:6][CH2:7][C@H:8]([OH:21])/[CH:9]=[CH:10]/[C@@H:11]1[C@@H:18]2[C@@H:14]([O:15][C:16](=[O:19])[CH2:17]2)[CH2:13][C@H:12]1[OH:20].[O:27]1[CH:32]=[CH:31][CH2:30][CH2:29][CH2:28]1.[C:33](=[O:36])(O)[O-].[Na+]>C1COCC1.O.C1(C)C=CC(S(O)(=O)=O)=CC=1>[O:27]1[CH2:28][CH2:29][CH2:30][CH2:31][CH:32]1[O:20][C@@H:12]1[CH2:13][C@@H:14]2[O:15][C:16](=[O:19])[CH2:17][C@@H:18]2[C@H:11]1/[CH:10]=[CH:9]/[C@@H:8]([O:21][CH:23]1[CH2:24][CH2:3][CH2:2][CH2:33][O:36]1)[CH2:7][O:6][C:5]1[CH:22]=[CH:23][CH:24]=[C:3]([C:2]([F:25])([F:1])[F:26])[CH:4]=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 3

HCID 80803,4-dihydro-2H-pyranHCID 516892Sodium BicarbonateHCID 12042328(+)-(3aR,4R,5R,6aS)-Hexahydro-5-hydroxy-4-[(1E,3R)-3-hydroxy-4-(3-trifluoromethyl)phenoxy-1-butenyl]-2H-cyclopenta[b]furan-2-one

生成物 1

HCID 117874872HCID 117874872、化合物収率 87.5%

試薬・触媒・溶媒 2

HCID 521998
p-Toluenesulfonic acid monohydrate
触媒
HCID 8028Tetrahydrofuran溶媒

実験手順

p-Toluenesulfonic acid monohydrate (0.35 g, 1.8 mmol) was added to a solution of (3aR,4R,5R,6aS)-4-((R,E)-4-(3-(trifluoromethyl)phenoxy)-3-hydroxybut-1-enyl)-hexahydro-5-hydroxycyclopenta[b]furan-2-one (15.0 g, 40.3 mmol) and 3,4-dihydro-2H-pyran (8.47 g, 100.7 mmol) in THF (200 mL) at room temperature and the mixture was stirred for 2.5 hr (TLC monitoring). Saturated aqueous solution of sodium bicarbonate (200 mL) was poured into the reaction mixture and the mixture was stirred for 5 minutes. The organic layer was separated and the aqueous layer was extracted with ethyl acetate (200 mL). The combined organic layers were dried over magnesium sulfate, filtered off solid and concentrated under reduced pressure to give 24.0 g of crude product. The crude product was purified by column chromatography and then concentrated under reduced pressure to provide 19.0 g of the titled compound (87.5% yield).

後処理

  1. stirringthe mixture was stirred for 5 minutes
  2. customThe organic layer was separated
  3. extractionthe aqueous layer was extracted with ethyl acetate (200 mL)
  4. dry with materialThe combined organic layers were dried over magnesium sulfate
  5. filtrationfiltered off solid
  6. concentrationconcentrated under reduced pressure
  7. customto give 24.0 g of crude product
  8. customThe crude product was purified by column chromatography
  9. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-1c7c69a790fd4f928c2b87e59a89d547
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09115109B2

反応ノート

読み込み中…

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