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Potassium Carbonate → Tert-butyl 5-(pyrazin-2-yl)picolinate

HRID 711289
ノート
印刷プレビュー

反応式

HRID 711289 の反応式
Br[C:2]1[CH:3]=[CH:4][C:5]([C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])=[N:6][CH:7]=1.CC1(C)C(C)(C)OB(B2OC(C)(C)C(C)(C)O2)O1.CC([O-])=O.[K+].C([O-])([O-])=O.[K+].[K+].Cl[C:45]1[CH:50]=[N:49][CH:48]=[CH:47][N:46]=1>C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2].C(Cl)Cl.C1COCC1>[C:11]([O:10][C:8](=[O:9])[C:5]1[CH:4]=[CH:3][C:2]([C:45]2[CH:50]=[N:49][CH:48]=[CH:47][N:46]=2)=[CH:7][N:6]=1)([CH3:14])([CH3:13])[CH3:12]
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

8

反応物 5

HCID 11430Potassium CarbonateHCID 73277ChloropyrazineHCID 517044Potassium AcetateHCID 2733548Bis(pinacolato)diboraneHCID 24997839tert-Butyl 5-bromopyridine-2-carboxylate

生成物 1

HCID 67208621Tert-butyl 5-(pyrazin-2-yl)picolinate

試薬・触媒・溶媒 2

HCID 178418807HCID 178418807、化合物触媒2 回
HCID 8028Tetrahydrofuran溶媒

反応条件

温度
80 °C

実験手順

The 250 mL flask was charged with tert-butyl 5-bromopicolinate 34h-4 (12.9 g, 50 mmol), 4,4,4′,4′,5,5,5′,5′-octamethyl-2,2′-bi(1,3,2-dioxaborolane) (13.9 g, 55 mmol), KOAc (9.8 g, 100 mmol), PdCl2(dppf)-CH2Cl2 adduct (0.408 g, 0.5 mmol) and THF (80 mL). The flask was sealed under nitrogen and the mixture was stirred at 80° C. for 24 hours. After completion of the reaction, it was cooled to room temperature and filtered through Celite. The filtrate was taken in 500 mL 4-necked RB flask and charged with aqueous K2CO3 solution (13.8 g in 100 ml Of water), 2-chloropyrazine (6.8 g, 60 mmol), and PdCl2(dppf)-CH2Cl2 adduct (0.204 g, 0.25 mmol). The reaction mixture was stirred at 64° C. for 2 h under nitrogen, cooled to room temperature and filtered through Celite. The filtrate was diluted with i-PrOAc (100 mL) and the aqueous layer separated. The organic layer was washed with water (2×100 mL), concentrated to ˜20 mL of volume and diluted with heptane (200 mL). The solid was collected by filtration, washed with heptane (50 mL), and dried at 40° C. to obtain 34h-1 as a pale yellow solid.

後処理

  1. customThe flask was sealed under nitrogen
  2. customAfter completion of the reaction, it
  3. temperaturewas cooled to room temperature
  4. filtrationfiltered through Celite
  5. stirringThe reaction mixture was stirred at 64° C. for 2 h under nitrogen
  6. temperaturecooled to room temperature
  7. filtrationfiltered through Celite
  8. additionThe filtrate was diluted with i-PrOAc (100 mL)
  9. customthe aqueous layer separated
  10. washThe organic layer was washed with water (2×100 mL)
  11. concentrationconcentrated to ˜20 mL of volume
  12. additiondiluted with heptane (200 mL)
  13. filtrationThe solid was collected by filtration
  14. washwashed with heptane (50 mL)
  15. customdried at 40° C.
  16. customto obtain 34h-1 as a pale yellow solid

出典と根拠

ORDレコード
ord-2e7a69acf6624149bd822dccc176c791
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09181235B2

反応ノート

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