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Borane;tetrahydrofuran → HCID 178419171, 화합물

HRID 2361551
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HRID 2361551 반응식
[CH3:1][N:2]([CH3:24])[C:3]1[C:8]([CH3:9])=[CH:7][C:6]([PH:10](=O)[C:11]2[CH:16]=[C:15]([CH3:17])[C:14]([N:18]([CH3:20])[CH3:19])=[C:13]([CH3:21])[CH:12]=2)=[CH:5][C:4]=1[CH3:23].[BH3:25].O1CCCC1>C1(C)C=CC=CC=1>[CH3:24][N:2]([CH3:1])[C:3]1[C:8]([CH3:9])=[CH:7][C:6]([PH:10][C:11]2[CH:16]=[C:15]([CH3:17])[C:14]([N:18]([CH3:19])[CH3:20])=[C:13]([CH3:21])[CH:12]=2)=[CH:5][C:4]=1[CH3:23].[BH3:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 2723981Borane;tetrahydrofuranHCID 178429638HCID 178429638, 화합물

생성물 1

HCID 178419171HCID 178419171, 화합물수율 65%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

Under an argon atmosphere, to a solution of bis(4-dimethylamino-3,5-dimethylphenyl)phosphine oxide (4.6 g, 14 mmoL) synthesized in Example 1 in toluene (30 mL) was added borane-tetrahydrofuran solution (71 mL, 5.4 equivalents) at room temperature over 2 hr. Then, silica gel (8.7 g, 10.8 equivalents) was added to the mixture, and the mixture was stirred at room temperature for 1.5 hr. The silica gel was removed by filtration, and the filtrate was concentrated under reduced pressure. The residue was purified by column chromatography (silica gel 20 g, toluene) and the residue was recrystallized from n-hexane to give the title compound (3.0 g, white crystals). yield 65%.

후처리

  1. additionThen, silica gel (8.7 g, 10.8 equivalents) was added to the mixture
  2. customThe silica gel was removed by filtration
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customThe residue was purified by column chromatography (silica gel 20 g, toluene)
  5. customthe residue was recrystallized from n-hexane

출처 및 근거

ORD 기록
ord-d98369f6a861487391372bcf42d5aff4
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08691718B2

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