HCID 57656231、化合物 → HCID 57656601、化合物

HRID 911593ノート

反応式

HRID 911593 の反応式
[C:1]([O:5][C:6]([NH:8][CH2:9][C:10]1[CH:15]=[CH:14][C:13]([CH:16]([OH:22])[CH2:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[CH:12][C:11]=1[F:23])=[O:7])([CH3:4])([CH3:3])[CH3:2]>O1CCOCC1.[O-2].[O-2].[Mn+4]>[C:1]([O:5][C:6]([NH:8][CH2:9][C:10]1[CH:15]=[CH:14][C:13]([C:16](=[O:22])[CH2:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[CH:12][C:11]=1[F:23])=[O:7])([CH3:4])([CH3:2])[CH3:3]

参加物

4

反応物 1

HCID 57656231HCID 57656231、化合物

生成物 1

HCID 57656601HCID 57656601、化合物収率 90%

試薬・触媒・溶媒 2

HCID 178418406HCID 178418406、化合物触媒HCID 312751,4-Dioxane溶媒

反応条件

温度
70 °C

実験手順

Add manganese dioxide (4.4 g, 50.6 mmol) to a solution of N-(tert-butoxycarbonyl)-2-fluoro-4-(1-hydroxy-3,3-dimethyl-butyl)-benzylamine (1.1 g, 3.38 mmol) in anhydrous 1,4-dioxane (45 mL) at room temperature. Heat the reaction mixture at 70° C. overnight. Filter the reaction mixture over Celite® and concentrate in vacuo. Purify by chromatography on silica gel eluting with hexane/EtOAc (9:1) to obtain the desired intermediate as an oil (980 mg, 90%).

後処理

  1. filtrationFilter the reaction mixture over Celite®
  2. concentrationconcentrate in vacuo
  3. customPurify by chromatography on silica gel eluting with hexane/EtOAc (9:1)

出典と根拠

ORDレコード
ord-ec5ad127a3c74b12874d46b808553864
出典データセット
uspto-grants-2011_09
特許番号
US08022062B2

反応ノート

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