Hydroxylamine → HCID 86661749、化合物

HRID 1024494ノート

反応式

HRID 1024494 の反応式
[O:1]1[C:7]2[CH:8]=[CH:9][C:10]([CH:12]=[CH:13][C:14](=O)[CH:15]([CH3:17])[CH3:16])=[CH:11][C:6]=2[O:5][CH2:4][CH2:3][CH2:2]1.C([O-])(=O)C.[Na+].[NH2:24][OH:25]>CO>[O:1]1[C:7]2[CH:8]=[CH:9][C:10]([CH:12]=[CH:13][C:14](=[N:24][OH:25])[CH:15]([CH3:17])[CH3:16])=[CH:11][C:6]=2[O:5][CH2:4][CH2:3][CH2:2]1

参加物

5

反応物 3

HCID 787HydroxylamineHCID 517045Sodium AcetateHCID 667262881-(3,4-dihydro-2H-1,5-benzodioxepine-7-yl)-4-methyl-1-penten-3-one

生成物 1

HCID 86661749HCID 86661749、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

145 mg 1-(3,4-dihydro-2H-1,5-benzodioxepine-7-yl)-4-methyl-1-penten-3-one was dissolved in methanol (20 ml), along with hydroxylamine hydrocholoride (244 mg) and sodium acetate (480 mg) and stirred in room temperature overnight. The reaction mixture was evaporated and the residue was dissolved in ethyl acetate (30 ml). After washing with 30 mL water and 30 mL Brine and drying with anhydrous sodium sulfate, the organic layer was concentrated under reduced pressure to yield crude product (M+1=262.1), that was used for next reaction.

後処理

  1. customThe reaction mixture was evaporated
  2. dissolutionthe residue was dissolved in ethyl acetate (30 ml)
  3. washAfter washing with 30 mL water and 30 mL Brine
  4. dry with materialdrying with anhydrous sodium sulfate
  5. concentrationthe organic layer was concentrated under reduced pressure
  6. customto yield crude product (M+1=262.1), that
  7. customwas used for next reaction

出典と根拠

ORDレコード
ord-43207cd4dd9c4166be3da12b75a911d6
出典データセット
uspto-grants-2014_05
特許番号
US08722896B2

反応ノート

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