Hydroxyamine hydrochloride → 4-[(2-Fluoro-5-trifluoromethyl-phenyl)-hydroxyiminomethyl]-piperidine-1-carboxylic acid tert-butyl ester

HRID 501313

反応式

HRID 501313 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([C:14](=O)[C:15]2[CH:20]=[C:19]([C:21]([F:24])([F:23])[F:22])[CH:18]=[CH:17][C:16]=2[F:25])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].Cl.[NH2:28][OH:29]>N1C=CC=CC=1>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([C:14]([C:15]2[CH:20]=[C:19]([C:21]([F:24])([F:23])[F:22])[CH:18]=[CH:17][C:16]=2[F:25])=[N:28][OH:29])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]

参加物

4

反応物 2

HCID 443297Hydroxyamine hydrochlorideHCID 588175444-(2-Fluoro-5-trifluoromethyl-benzoyl)-piperidine-1-carboxylic acid tert-butyl ester

生成物 1

HCID 724345474-[(2-Fluoro-5-trifluoromethyl-phenyl)-hydroxyiminomethyl]-piperidine-1-carboxylic acid tert-butyl ester

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A solution of 4-(2-fluoro-5-trifluoromethyl-benzoyl)-piperidine-1-carboxylic acid tert-butyl ester (59, 0.013M) in pyridine (25 mL) was treated with hydroxylamine hydrochloride (1.11 g, 0.015 M-1.2 eq). The reaction was stirred under N2 at room temperature for 14 hours and then poured onto ice water (250 mL). The mixture was stirred at 0° C. for 1 hour, the product was then filtered off, washed with cold water (3×15 mL) and dried in a vacuum oven at 50° C. A white solid was obtained (5.03 g, 97%).

後処理

  1. additionpoured onto ice water (250 mL)
  2. stirringThe mixture was stirred at 0° C. for 1 hour
  3. filtrationthe product was then filtered off
  4. washwashed with cold water (3×15 mL)
  5. customdried in a vacuum oven at 50° C
  6. customA white solid was obtained (5.03 g, 97%)

出典と根拠

ORDレコード
ord-d3befe8109454906845c3d380e924555
出典データセット
uspto-grants-2010_08
特許番号
US07772252B2

関連ノート

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