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三乙胺 → HCID 59255279,化合物

HRID 1691237
笔记
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反应方程式

HRID 1691237 反应方程式
[N+:1]([CH2:4][CH2:5][C:6]1[CH:18]=[CH:17][C:9]([O:10][C:11]2[CH:12]=[N:13][CH:14]=[CH:15][CH:16]=2)=[CH:8][CH:7]=1)([O-:3])=O.C[O-].[Li+].C(=O)(O)[O-].[Na+].[C:27]([C:29]1[C:30]([NH2:36])=[N:31][C:32]([NH2:35])=[CH:33][CH:34]=1)#[CH:28].C(N(CC)CC)C>[Ti](Cl)(Cl)(Cl)Cl.O.O1CCCC1.C(OCC)(=O)C.CO>[N:13]1[CH:14]=[CH:15][CH:16]=[C:11]([O:10][C:9]2[CH:17]=[CH:18][C:6]([CH2:5][C:4]3[CH:28]=[C:27]([C:29]4[C:30]([NH2:36])=[N:31][C:32]([NH2:35])=[CH:33][CH:34]=4)[O:3][N:1]=3)=[CH:7][CH:8]=2)[CH:12]=1
参与物实验过程后处理来源与证据反应笔记

参与物

11

反应物 5

HCID 8471三乙胺HCID 516892碳酸氢钠HCID 4177230甲醇锂HCID 552816763-乙炔基吡啶-2,6-二胺HCID 592552763-(4-(2-Nitro-ethyl)-phenoxy)-pyridine

产物 1

HCID 59255279HCID 59255279,化合物收率 15.8%

试剂、催化剂与溶剂 5

HCID 24193
四氯化钛
催化剂
HCID 887Methanol溶剂
HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂
HCID 8028四氢呋喃溶剂
HCID 8857乙酸乙酯溶剂

实验过程

To a methanol (10.0 mL) solution of 3-(4-(2-nitro-ethyl)-phenoxy)-pyridine (819 mg, 3.35 mmol) described in Manufacturing Example 76-1-3 was added lithium methoxide (254 mg, 6.70 mmol), which was stirred for 30 minutes at room temperature. The reaction mixture was concentrated under a reduced pressure, and anhydrous dichloromethane (15.0 mL) and anhydrous tetrahydrofuran (7.00 mL) were added to the residue. Titanium (IV) chloride (1.18 mL, 10.7 mmol) was added dropwise to the reaction mixture on a dry ice-ethanol bath (−78° C.), after which the system was stirred for 30 minutes at room temperature. Aqueous sodium bicarbonate and ethyl acetate were added to the reaction mixture on an ice bath (0° C.), and the mixture was filtered through a Celite pad. The organic layer of the filtrate was extracted with ethyl acetate, and this organic layer was washed with water and saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate, and the filtrate was concentrated under a reduced pressure, which gave a crude product (400 mg). To a tetrahydrofuran (5.00 mL) solution of 3-ethynyl-pyridin-2,6-diamine (40.0 mg, 0.300 mmol) described in Manufacturing Example 13-1-3 and this crude product (150 mg) was added triethylamine (125 μL, 0.900 mmol), which was stirred for 3 hours at 60° C. Water was added to the reaction solution at room temperature, which was extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium chloride and dried over anhydrous magnesium sulfate, and the solvent was evaporated under a reduced pressure. The residue was purified by NH silica gel column chromatography (ethyl acetate:heptane=3:1→5:1) to obtain the title compound (17.0 mg, 15.8%).

后处理

  1. concentrationThe reaction mixture was concentrated under a reduced pressure, and anhydrous dichloromethane (15.0 mL) and anhydrous tetrahydrofuran (7.00 mL)
  2. additionwere added to the residue
  3. stirringafter which the system was stirred for 30 minutes at room temperature
  4. filtrationthe mixture was filtered through a Celite pad
  5. extractionThe organic layer of the filtrate was extracted with ethyl acetate
  6. washthis organic layer was washed with water and saturated aqueous sodium chloride
  7. dry with materialdried over anhydrous magnesium sulfate
  8. concentrationthe filtrate was concentrated under a reduced pressure, which
  9. customgave a crude product (400 mg)
  10. stirringwas stirred for 3 hours at 60° C
  11. extractionwhich was extracted with ethyl acetate
  12. washThe organic layer was washed with saturated aqueous sodium chloride
  13. dry with materialdried over anhydrous magnesium sulfate
  14. customthe solvent was evaporated under a reduced pressure
  15. customThe residue was purified by NH silica gel column chromatography (ethyl acetate:heptane=3:1→5:1)

来源与证据

ORD记录
ord-82aaf436acfd4bc9b29b9544e34e41a0
来源数据集
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
专利号
US08153662B2

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