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Hydrochloric Acid → (R)-1-(6-(4-(4-fluorophenoxy)phenyl)pyridin-2-yl)-2,3-

HRID 1500200
ノート
印刷プレビュー

反応式

HRID 1500200 の反応式
CC1(C)[O:6][C@@H:5]([C:7]([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([C:15]3[CH:20]=[CH:19][C:18]([O:21][C:22]4[CH:27]=[CH:26][C:25]([F:28])=[CH:24][CH:23]=4)=[CH:17][CH:16]=3)[N:10]=2)=[O:8])[CH2:4][O:3]1.C(Cl)Cl.CO.Cl.O>O1CCOCC1.C(Cl)Cl.C([O-])(O)=O.[Na+]>[F:28][C:25]1[CH:24]=[CH:23][C:22]([O:21][C:18]2[CH:19]=[CH:20][C:15]([C:11]3[N:10]=[C:9]([C:7](=[O:8])[C@H:5]([OH:6])[CH2:4][OH:3])[CH:14]=[CH:13][CH:12]=3)=[CH:16][CH:17]=2)=[CH:27][CH:26]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 21226129Dichloromethane methanolHCID 89822495(R)-(2,2-dimethyl-1,3-dioxolan-4-yl)(6-(4-(4-fluorophenoxy)phenyl)pyridin-2-yl)methanone

生成物 1

HCID 71722102(R)-1-(6-(4-(4-fluorophenoxy)phenyl)pyridin-2-yl)-2,3-収率 28%

試薬・触媒・溶媒 3

HCID 6344
Dichloromethane
溶媒
HCID 312751,4-Dioxane溶媒
HCID 516892Sodium Bicarbonate溶媒

実験手順

To a solution of (R)-(2,2-dimethyl-1,3-dioxolan-4-yl)(6-(4-(4-fluorophenoxyl)phenyl)pyridin-2-yl)methanone (0.621, g, 1.58, mmol) in an 85:15, mixture of DCM/MeOH (10, mL) was added 4M HCl in dioxane (2, mL, 8, mmol). After stirring overnight 0.5, mL, water was added to the reaction. After 3, more hours the reaction was diluted with 50, mL DCM and solid NaHCO3, was added. After the bubbling subsided, the reaction mixture was dried over Na2SO4, filtered, and evaporated in vacuo to a residue. The residue was chromatographed over silica gel with 10-75% acetone in hexanes. The product fractions were isolated and evaporated in vacuo. The residue was dissolved in acetone, evaporated in vacuo, dissolved in EtOAc and hexanes, evaporated in vacuo, treated with hexanes, and evaporated in vacuo. The material was dried under vacuum at 50° C. to give the product (R)-1-(6-(4-(4-fluorophenoxy)phenyl)pyridin-2-yl)-2,3-dihydroxypropan-1-one as a glassy orange solid (0.155, g, 0.44, mmol, 28% yield). LC/MS: m/z=354.1, [M+H]+, ; 1H NMR (400, MHz, DMSO-d6): 8.23-8.17, (3 H, m), 8.08, (1 H, t, J=7.9, Hz), 7.88, (1 H, dd, J=7.7, Hz, 0.9, Hz), 7.32-7.25, (2 H, m), 7.20-7.15, (2 H, m), 7.12, (2 H, d, J=9.0, Hz), 5.54-5.49, (1 H, m), 5.09, (1 H, d, J=7.0, Hz), 4.78, (1 H, t, J=5.5, Hz), 3.93-3.81, (2 H, m). Unless otherwise indicated all 1H NMR chemical shifts reported herein are denoted by the delta (δ) scale.

後処理

  1. additionwas added
  2. dry with materialthe reaction mixture was dried over Na2SO4
  3. filtrationfiltered
  4. customevaporated in vacuo to a residue
  5. customThe residue was chromatographed over silica gel with 10-75% acetone in hexanes
  6. customThe product fractions were isolated
  7. customevaporated in vacuo
  8. dissolutionThe residue was dissolved in acetone
  9. customevaporated in vacuo
  10. dissolutiondissolved in EtOAc
  11. customhexanes, evaporated in vacuo
  12. additiontreated with hexanes
  13. customevaporated in vacuo
  14. customThe material was dried under vacuum at 50° C.

出典と根拠

ORDレコード
ord-a49d85b2d3f143c884ef14301c155784
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09206127B2

反応ノート

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