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Hydrogen Peroxide → HCID 23028618、化合物

HRID 748865
ノート
印刷プレビュー

反応式

HRID 748865 の反応式
OO.Cl[C:4]1C(C(SC2C=NC(Cl)=CC=2)C2C=CN=CC=2)=NC(Cl)=CC=1.C(OCC)(=O)C.[Si:32]([O:39][CH2:40][CH2:41][CH:42](C)[CH:43]([C:54]1[CH:59]=[C:58]([F:60])[CH:57]=[CH:56][C:55]=1[F:61])[S:44]([C:47]1[CH:52]=[CH:51][C:50]([Cl:53])=[CH:49][CH:48]=1)(=[O:46])=[O:45])([C:35]([CH3:38])([CH3:37])[CH3:36])([CH3:34])[CH3:33]>CO.CCCCCC>[Si:32]([O:39][CH:40]([CH3:4])[CH2:41][CH2:42][CH:43]([C:54]1[CH:59]=[C:58]([F:60])[CH:57]=[CH:56][C:55]=1[F:61])[S:44]([C:47]1[CH:48]=[CH:49][C:50]([Cl:53])=[CH:51][CH:52]=1)(=[O:46])=[O:45])([C:35]([CH3:36])([CH3:38])[CH3:37])([CH3:33])[CH3:34]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 784Hydrogen PeroxideHCID 8857Ethyl Acetate2 回HCID 231147773,6-Dichloro-2-[(6-chloropyridin-3-ylthio)(pyridin-4-yl)methyl]pyridineHCID 59750761HCID 59750761、化合物

生成物 1

HCID 23028618HCID 23028618、化合物収率 20.4%

試薬・触媒・溶媒 2

HCID 887
Methanol
溶媒
HCID 8058Hexane溶媒

実験手順

A 31% aqueous hydrogen peroxide solution (2 ml) and hexaammonium heptamolybdate tetrahydrate (30 mg) were added to a solution of 3,6-dichloro-2-[(6-chloropyridin-3-ylthio) (pyridin-4-yl)methyl]pyridine (82 mg, 0.24 mmol) in methanol (4 ml). The resulting mixture was stirred at room temperature for 2 hours. Ethyl acetate was added to the reaction mixture. After washing with a saturated aqueous solution of sodium bicarbonate, the organic layer was dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated under reduced pressure. The residue was subjected to flash chromatography on a silica gel column. A fraction obtained from the elution portion with hexane:ethyl acetate=3:2 was concentrated under reduced pressure, whereby the title compound A (41 mg, 0.098 mmol, 46%) was obtained. A fraction obtained from the elution portion with hexane:ethyl acetate=1:1 was concentrated under reduced pressure, whereby the title compound B (isomer A) (low polarity) (8 mg, 0.020 mmol, 9%) and the title compound B (isomer B) (high polarity) (8 mg, 0.020 mmol, 9%) were obtained, respectively each as a white solid.

後処理

  1. washAfter washing with a saturated aqueous solution of sodium bicarbonate
  2. dry with materialthe organic layer was dried over anhydrous sodium sulfate
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. customA fraction obtained from the elution portion with hexane
  6. customwas obtained
  7. concentrationethyl acetate=1:1 was concentrated under reduced pressure, whereby the title compound B (isomer A) (low polarity) (8 mg, 0.020 mmol, 9%)

出典と根拠

ORDレコード
ord-273f7493e00542ffb7aa237e61b41234
出典データセット
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07399775B2

反応ノート

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