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氢化钠 → 1-(Pyridin-3-ylsulfonyl)-5-[2-(trifluoromethyl)phenyl]-1H-pyrrole-3-carbaldehyde

HRID 554331
笔记
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反应方程式

HRID 554331 反应方程式
[F:1][C:2]([F:17])([F:16])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]1[NH:13][CH:12]=[C:11]([CH:14]=[O:15])[CH:10]=1.[H-].[Na+].C1OCCOCCOCCOCCOC1.Cl.[N:36]1[CH:41]=[CH:40][CH:39]=[C:38]([S:42](Cl)(=[O:44])=[O:43])[CH:37]=1>O1CCCC1.[Cl-].[Na+].O>[N:36]1[CH:41]=[CH:40][CH:39]=[C:38]([S:42]([N:13]2[C:9]([C:4]3[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=3[C:2]([F:16])([F:1])[F:17])=[CH:10][C:11]([CH:14]=[O:15])=[CH:12]2)(=[O:44])=[O:43])[CH:37]=1
参与物实验过程后处理来源与证据反应笔记

参与物

7

反应物 4

HCID 24758氢化钠HCID 3633615-冠醚-5HCID 12571517吡啶-3-磺酰氯盐酸盐HCID 862327755-[2-(Trifluoromethyl)phenyl]-1H-pyrrole-3-carbaldehyde

产物 1

HCID 866207601-(Pyridin-3-ylsulfonyl)-5-[2-(trifluoromethyl)phenyl]-1H-pyrrole-3-carbaldehyde收率 100%

试剂、催化剂与溶剂 2

HCID 8028
四氢呋喃
溶剂
HCID 57417360Sodium chloride; water溶剂

实验过程

To a solution (36 mL) of 5-[2-(trifluoromethyl)phenyl]-1H-pyrrole-3-carbaldehyde (240 mg) in tetrahydrofuran was added sodium hydride (60% in oil, 201 mg) at room temperature and the mixture was stirred for 30 min. 15-Crown-5 (1.11 g) was added dropwise and the mixture was stirred for 30 min. Pyridine-3-sulfonyl chloride hydrochloride (537 mg) was added, and the mixture was further stirred for 3 hr. Saturated brine was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: hexane-ethyl acetate=4:1→2:3) and crystallized from diisopropyl ether to give the title compound as colorless crystals (yield 380 mg, about 100%).

后处理

  1. stirringthe mixture was stirred for 30 min
  2. stirringthe mixture was further stirred for 3 hr
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe extract was washed with saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (eluent: hexane-ethyl acetate=4:1→2:3)
  8. customcrystallized from diisopropyl ether

来源与证据

ORD记录
ord-88c6a889dea7426f878b10dc3d46b61a
来源数据集
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
专利号
US08048909B2

反应笔记

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本页导航参与物实验过程后处理来源与证据反应笔记