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碳酸氢铯 → 2-Dimethylamino-6-vinyl-isonicotinic acid tert-butyl ester

HRID 1908753
笔记
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反应方程式

HRID 1908753 反应方程式
[C:1]([O:5][C:6](=[O:17])[C:7]1[CH:12]=[C:11]([N:13]([CH3:15])[CH3:14])[N:10]=[C:9](Cl)[CH:8]=1)([CH3:4])([CH3:3])[CH3:2].C([O-])([O-])=O.[Cs+].[Cs+].B1(C=C)OB([CH:30]=[CH2:31])OB(C=C)O1.C1C=CN=CC=1>O1CCOCC1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[C:1]([O:5][C:6](=[O:17])[C:7]1[CH:8]=[C:9]([CH:30]=[CH2:31])[N:10]=[C:11]([N:13]([CH3:15])[CH3:14])[CH:12]=1)([CH3:4])([CH3:3])[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

6

反应物 3

HCID 10796碳酸氢铯HCID 2734806乙烯硼酐吡啶络合物HCID 866405942-Chloro-6-dimethylamino-isonicotinic acid tert-butyl ester

产物 1

HCID 670269302-Dimethylamino-6-vinyl-isonicotinic acid tert-butyl ester收率 118.8%

试剂、催化剂与溶剂 2

HCID 9811564三(二亚苄基丙酮)二钯催化剂
HCID 31275
1,4-二氧六环
溶剂

反应条件

温度
100 °C

实验过程

To a solution of 2-chloro-6-dimethylamino-isonicotinic acid tert-butyl ester (770 mg, 3.00 mmol) in dioxane (45 mL), Cs2CO3 (1270 mg, 3.90 mmol) followed by P(tert.-Bu)3 (30 mg, 0.15 mmol) and 2,4,6-trivinylcyclotriboroxane pyridine complex (722 mg, 3.00 mmol, prepared according to F. Kerins, D. F. O'Shea J. Org. Chem. 67 (2002) 4968-4971) is added. The mixture is degassed and put under argon before Pd2(dba)3 (82 mg, 0.09 mmol) is added. The mixture is stirred at 100° C. for 15 h before it is cooled to rt and filtered over a short silica gel pad eluting with DCM. The filtrate is concentrated and purified on prep. TLC plates with DCM to give 2-dimethylamino-6-vinyl-isonicotinic acid tert-butyl ester (885 mg) as a red to brownish resin; LC-MS: tR=0.82 min, [M+1]+=249.37.

后处理

  1. customThe mixture is degassed
  2. additionis added
  3. temperatureis cooled to rt
  4. filtrationfiltered over a short silica gel pad
  5. washeluting with DCM
  6. concentrationThe filtrate is concentrated
  7. custompurified on prep

来源与证据

ORD记录
ord-55ab860aa8ae49b9bde8af746e6dca62
来源数据集
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
专利号
US08598208B2

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