Triethylamine → N-(3,4-dihydro-2H-naphthalen-1-ylidene)hydroxylamine

HRID 448878

反応式

HRID 448878 の反応式
[CH2:1]1[CH2:11][C:9](=O)[C:8]2[C:3](=[CH:4][CH:5]=[CH:6][CH:7]=2)[CH2:2]1.Cl.[NH2:13][OH:14].C(N(CC)CC)C>CO>[C:9]1(=[N:13][OH:14])[C:8]2[C:3](=[CH:4][CH:5]=[CH:6][CH:7]=2)[CH2:2][CH2:1][CH2:11]1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 107241-TetraloneHCID 443297Hydroxyamine hydrochloride

生成物 1

HCID 76876N-(3,4-dihydro-2H-naphthalen-1-ylidene)hydroxylamine収率 108.7%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of α-tetralone (10 g, 68.5 mmol) in anhydrous MeOH (175 mL), hydroxylamine hydrochloride (7.6 g, 109.6 mmol) and triethylamine (15.3 mL, 109.6 mmol) were added. The mixture was stirred at room temperature for 16 hrs, followed by removal of the solvent in vacuo. The residue was dissolved in DCM, washed with water and brine, dried (Na2SO4), filtered and concentrated in vacuo to yield crude 3,4-dihydro-2H-naphthalen-1-one oxime (12 g). MS [M+H]+: 162.1; tR=2.03 min. (method 1)

後処理

  1. customfollowed by removal of the solvent in vacuo
  2. dissolutionThe residue was dissolved in DCM
  3. washwashed with water and brine
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-e6abb06940f34a21842540b7f830e82c
出典データセット
uspto-grants-2013_07
特許番号
US08481738B2

関連ノート

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