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O-Methylhydroxylamine hydrochloride → HCID 86015016、化合物

HRID 451604
ノート
印刷プレビュー

反応式

HRID 451604 の反応式
[N:1]1([C:7]2[CH:8]=[C:9]3[C:13](=[CH:14][CH:15]=2)[C:12](=O)[CH2:11][CH2:10]3)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.Cl.[CH3:18][O:19][NH2:20]>N1C=CC=CC=1>[CH3:18][O:19][N:20]=[C:12]1[C:13]2[C:9](=[CH:8][C:7]([N:1]3[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]3)=[CH:15][CH:14]=2)[CH2:10][CH2:11]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 521874O-Methylhydroxylamine hydrochlorideHCID 222283835-(Piperidin-1-yl)-2,3-dihydro-1H-inden-1-one

生成物 1

HCID 86015016HCID 86015016、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

5-Piperidin-1-ylindan-1-one (4.31 g, 20 mmol) in pyridine (20 ml) was treated with methoxyamine hydrochloride (1.84 g, 22 mmol). After stirring at ambient temperature for 40 hours, the solvent was removed under vacuum and the residue taken in water and extracted with diethyl ether. The combined organic layers were washed with water, dried with magnesium sulfate, filtered, and the filtrate was removed under vacuum to provide the title compound which was used without further purification. 1H NMR (CDCl3) δ 1.56-1.73 (m, 6H), 2.78-2.89 (m, 1H), 2.91-3.02 (m, 1H), 3.20-3.30 (m, 2H), 3.95 (s, 3H), 6.78 (m, 1H), 6.84 (m, 1H), 7.54 (d, 1H); MS (DCI): 245 (M+H)+.

後処理

  1. customthe solvent was removed under vacuum
  2. extractionextracted with diethyl ether
  3. washThe combined organic layers were washed with water
  4. dry with materialdried with magnesium sulfate
  5. filtrationfiltered
  6. customthe filtrate was removed under vacuum

出典と根拠

ORDレコード
ord-cd89ff2c04054f728c8e03f351a72642
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08487116B2

反応ノート

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