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三乙胺 → 2-tert-Butyl-4-[(3S)-3-(dimethylamino)pyrrolidin-1-yl]-6-methyl-6-phenyl-1,3-benzoxazole-7-carbonitrile

HRID 17529
笔记
打印预览

反应方程式

HRID 17529 反应方程式
[C:1]([C:5]1[O:6][C:7]2[C:13]([C:14]#[N:15])=[C:12]([CH3:16])[C:11](C3C=CC=CC=3)=[C:10](F)[C:8]=2[N:9]=1)([CH3:4])([CH3:3])[CH3:2].C(N([CH2:29][CH3:30])CC)C.[CH3:31][N:32]([CH3:38])[C@H:33]1[CH2:37][CH2:36][NH:35][CH2:34]1.C(=O)([O-])O.[Na+]>CS(C)=O.C(OCC)(=O)C>[C:1]([CH:5]1[N:9]=[C:8]2[C:10]([N:35]3[CH2:36][CH2:37][C@H:33]([N:32]([CH3:38])[CH3:31])[CH2:34]3)=[CH:11][C:12]([CH3:16])([C:30]3[CH:29]=[CH:10][CH:8]=[CH:7][CH:13]=3)[C:13]([C:14]#[N:15])=[C:7]2[O:6]1)([CH3:3])([CH3:4])[CH3:2]
参与物反应条件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 8471三乙胺HCID 516892碳酸氢钠HCID 7019156(3S)-(-)-3-(二甲氨基)吡咯烷HCID 68584886HCID 68584886,化合物

产物 1

HCID 685848532-tert-Butyl-4-[(3S)-3-(dimethylamino)pyrrolidin-1-yl]-6-methyl-6-phenyl-1,3-benzoxazole-7-carbonitrile收率 87%

试剂、催化剂与溶剂 2

HCID 679
二甲基亚砜
溶剂
HCID 8857乙酸乙酯溶剂

反应条件

温度
90 °C

实验过程

2-tert-Butyl-4-fluoro-6-methyl-5-phenyl-1,3-benzoxazole-7-carbonitrile (I-239) (105 mg, 0.34 mmol) was dissolved in dimethyl sulfoxide (2 ml), and at room temperature, triethylamine (95 μl, 0.68 mmol) and (3S)-3-(dimethylamino)pyrrolidine (65 μl, 0.51 mmol) were added. The solution was stirred under nitrogen atmosphere at 90° C. for 6 hours. After cooling to room temperature, the reaction liquid was fractionated with ethyl acetate and an aqueous saturated sodium hydrogencarbonate solution. The aqueous layer was further extracted with ethyl acetate. The organic layers were combined, washed with saturated brine, then dried over anhydrous sodium sulfate. The insoluble matter was separated by filtration, then the solvent was evaporated away, and the resulting residue was purified by middle-pressure liquid chromatography (eluent, chloroform:methanol=98:2) to obtain the entitled compound (119 mg, 87%) as a pale yellow solid.

后处理

  1. temperatureAfter cooling to room temperature
  2. customthe reaction liquid
  3. extractionThe aqueous layer was further extracted with ethyl acetate
  4. washwashed with saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe insoluble matter was separated by filtration
  7. customthe solvent was evaporated away
  8. customthe resulting residue was purified by middle-pressure liquid chromatography (eluent, chloroform:methanol=98:2)

来源与证据

ORD记录
ord-64761abc99b847f49d8543de2f6a3e16
来源数据集
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
专利号
US07737166B2

反应笔记

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本页导航参与物反应条件实验过程后处理来源与证据反应笔记