HCID 57656231, 화합물 → HCID 57656601, 화합물

HRID 911593노트

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HRID 911593 반응식
[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]

참가 물질

4

반응물 1

HCID 57656231HCID 57656231, 화합물

생성물 1

HCID 57656601HCID 57656601, 화합물수율 90%

시약·촉매·용매 2

HCID 178418406HCID 178418406, 화합물촉매HCID 312751,4-Dioxane용매

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온도
70 °C

실험 절차

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%).

후처리

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

출처 및 근거

ORD 기록
ord-ec5ad127a3c74b12874d46b808553864
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08022062B2

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