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Cesium carbonate → 6-Isopropoxy-5-methyl-nicotinic acid isopropyl ester

HRID 1908758
ノート
印刷プレビュー

反応式

HRID 1908758 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

9

反応物 3

HCID 10796Cesium carbonateHCID 574072TrimethylboroxineHCID 22985641Isopropyl 5-chloro-6-isopropoxynicotinate

生成物 1

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

試薬・触媒・溶媒 5

HCID 83681Tris(1,1-dimethylethyl)phosphine触媒
HCID 9811564
Bis(dibenzylideneacetone)palladium
触媒
HCID 962Water溶媒
HCID 312751,4-Dioxane溶媒
HCID 516892Sodium Bicarbonate溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-17b79141a5b5470594ca94eb5abfd537
出典データセット
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08598208B2

反応ノート

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