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Methanesulfonamide → HCID 66634221、化合物

HRID 537385
ノート
印刷プレビュー

反応式

HRID 537385 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1/[CH:8]=[CH:9]/[CH3:10].CC[C@H]1[C@H]2C[C@H]([C@H](OC3C4C(=CC=CC=4)C(O[C@H](C4C=CN=C5C=4C=C(OC)C=C5)[C@@H]4N5C[C@H](CC)[C@@H](CC5)C4)=NN=3)C3C=CN=C4C=3C=C([O:32]C)C=C4)N(CC2)C1.CS(N)(=O)=O.CC(O)(C)C.[OH2:79]>>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C@@H:8]([OH:32])[C@H:9]([OH:79])[CH3:10]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 72879MethanesulfonamideHCID 14419677(E)-1-Chloro-2-propenylbenzeneHCID 510036741-((1R)-((2R,4R,5S)-5-ethylquinuclidin-2-yl)(6-methoxyquinolin-4-yl)methoxy)-4-((1R)-((2R,4S,5R)-5-ethylquinuclidin-2-yl)(6-methoxyquinolin-4-yl)methoxy)phthalazineHCID 714019492-Methylpropan-2-ol--water (1/1)

生成物 1

HCID 66634221HCID 66634221、化合物収率 90%

実験手順

1-(2-chlorophenyl)-trans-1-propene (2.5 g, Preparation Example 1) was dissolved in 50 mL of the mixture of t-BuOH/H2O (1:1 (V/V)). At 0° C., AD-mix-α (Aldrich, U.S.A.) (23.5 g) and methane sulfone amide (CH3SO2NH2, 1.27 g, 0.013 mol) were added thereto and stirred for overnight. When the reaction was completed, the obtained product was washed with an aqueous solution of sodium sulfite (Na2SO3) and ethylacetate (EA). Then, the organic layer was dehydrated with anhydrous magnesium sulfate (MgSO4), filtrated, and concentrated under reduced pressure. The concentrated residue was purified by a silica gel column chromatography to produce the title compound (2.96 g, yield 90%).

後処理

  1. washthe obtained product was washed with an aqueous solution of sodium sulfite (Na2SO3) and ethylacetate (EA)
  2. filtrationfiltrated
  3. concentrationconcentrated under reduced pressure
  4. customThe concentrated residue was purified by a silica gel column chromatography

出典と根拠

ORDレコード
ord-6f6223f9096b46d79c6e20853e4b6878
出典データセット
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08859817B2

反応ノート

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