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Sodium Carbonate → Methyl 4-(2-Chloro-5-fluoro-4-pyrimidinyl)benzoate

HRID 968694
ノート
印刷プレビュー

反応式

HRID 968694 の反応式
[Cl:1][C:2]1[N:7]=[C:6](Cl)[C:5]([F:9])=[CH:4][N:3]=1.COB([C:14]1[CH:19]=[CH:18][C:17]([C:20]([OH:22])=[O:21])=[CH:16][CH:15]=1)O.[C:23]([O-])([O-])=O.[Na+].[Na+]>COCCOC.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH3:23][O:22][C:20](=[O:21])[C:17]1[CH:16]=[CH:15][C:14]([C:6]2[C:5]([F:9])=[CH:4][N:3]=[C:2]([Cl:1])[N:7]=2)=[CH:19][CH:18]=1
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

6

反応物 3

HCID 10340Sodium CarbonateHCID 2507052,4-Dichloro-5-fluoropyrimidineHCID 669046664-Carboxybenzeneboronic acid methyl ester

生成物 1

HCID 85941984Methyl 4-(2-Chloro-5-fluoro-4-pyrimidinyl)benzoate収率 46%

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒
HCID 8071
1,2-Dimethoxyethane
溶媒

反応条件

温度
85 °C

実験手順

To a solution of 2,4-dichloro-5-fluoropyrimidine (0.478 g, 2.86 mmol) and 4-carboxyphenyl boronic acid methyl ester (0.516 g, 2.86 mmol) in 5 mL of ethyleneglycol dimethyl ether was added Pd(PPh3)4 under argon, followed by 2N Na2CO3 and the resulting mixture purged with argon for 2 minutes. The resulting mixture was sealed and heated at 85° C. overnight. After 18 hours, the reaction was diluted with 20 mL of ethyl acetate and washed with H2O. The organic layer was concentrated and purified by chromatography (Silica, 10% ethyl acetate in hexanes) to afford 4-(2-chloro-5-fluoropyrimidin-4-yl)-benzoic acid methyl ester (0.35 g, 46%) as a white solid. LCMS: ES+=267.

後処理

  1. customthe resulting mixture purged with argon for 2 minutes
  2. customThe resulting mixture was sealed
  3. additionthe reaction was diluted with 20 mL of ethyl acetate
  4. washwashed with H2O
  5. concentrationThe organic layer was concentrated
  6. custompurified by chromatography (Silica, 10% ethyl acetate in hexanes)

出典と根拠

ORDレコード
ord-278f07dca0664cd1a90f4aeb191c38d4
出典データセット
uspto-grants-2007_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07304071B2

反応ノート

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