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碳酸氢铯 → 6-Isopropoxy-5-methyl-nicotinic acid isopropyl ester

HRID 1908758
笔记
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反应方程式

HRID 1908758 反应方程式
[CH:1]([O:4][C:5](=[O:17])[C:6]1[CH:11]=[C:10](Cl)[C:9]([O:13][CH:14]([CH3:16])[CH3:15])=[N:8][CH:7]=1)([CH3:3])[CH3:2].[CH3:18]B1OB(C)OB(C)O1.C([O-])([O-])=O.[Cs+].[Cs+]>O1CCOCC1.O.C([O-])(O)=O.[Na+].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(P(C(C)(C)C)C(C)(C)C)(C)(C)C>[CH:1]([O:4][C:5](=[O:17])[C:6]1[CH:11]=[C:10]([CH3:18])[C:9]([O:13][CH:14]([CH3:16])[CH3:15])=[N:8][CH:7]=1)([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

9

反应物 3

HCID 10796碳酸氢铯HCID 574072三甲基环三硼氧烷HCID 22985641Isopropyl 5-chloro-6-isopropoxynicotinate

产物 1

HCID 670269796-Isopropoxy-5-methyl-nicotinic acid isopropyl ester收率 41.6%

试剂、催化剂与溶剂 5

HCID 83681三叔丁基膦催化剂
HCID 9811564
三(二亚苄基丙酮)二钯
催化剂
HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂
HCID 312751,4-二氧六环溶剂
HCID 516892碳酸氢钠溶剂

反应条件

温度
100 °C

实验过程

To a solution of 5-chloro-6-isopropoxy-nicotinic acid isopropyl ester (235 mg, 0.912 mmol) in dioxane (5 mL), 2,4,6-trimethyl-cyclotriboroxane (114 mg, 0.912 mmol), Cs2CO3 (386 mg, 1.19 mmol) and tri-tert.-butylphosphine (7.4 mg, 36 μmol) is added. The mixture is degassed and put under argon before Pd2(dba)3 (17 mg, 18 μmol) is added. The mixture is stirred at 100° C. for 18 h. The mixture is cooled to rt, diluted with water and sat. aq. NaHCO3-solution and extracted with EA. The org. extract is dried over MgSO4, filtered and concentrated. The crude product is purified on prep. TLC plates with heptane:EA 9:1 to give 6-isopropoxy-5-methyl-nicotinic acid isopropyl ester (90 mg) as a colourless oil; LC-MS: tR=1.08 min; [M+1]+=238.08; 1H NMR (CDCl3): δ 1.35-1.41 (m, 12H), 2.20 (s, 3H), 5.20-5.30 (m, 1H), 5.37-5.48 (m, 1H), 7.95 (s, 1H), 8.67 (s, 1H). The title compound can be obtained by hydrolising 6-isopropoxy-5-methyl-nicotinic acid isopropyl ester according to the procedure given in step d) of the preparation of 5,6-diisobutyl-nicotinic acid.

后处理

  1. customThe mixture is degassed
  2. additionis added
  3. temperatureThe mixture is cooled to rt
  4. extractionextracted with EA
  5. extractionextract
  6. dry with materialis dried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customThe crude product is purified on prep

来源与证据

ORD记录
ord-17b79141a5b5470594ca94eb5abfd537
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