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Chloroform → Ethyl 4-(4-chloro-2-methoxyphenyl)-1-methyl-1H-pyrrole-2-carboxylate

HRID 1498912
ノート
印刷プレビュー

反応式

HRID 1498912 の反応式
Br[C:2]1[CH:3]=[C:4]([C:8]([O:10][CH2:11][CH3:12])=[O:9])[N:5]([CH3:7])[CH:6]=1.C(=O)([O-])[O-].[Na+].[Na+].[Cl:19][C:20]1[CH:25]=[CH:24][C:23](B(O)O)=[C:22]([O:29][CH3:30])[CH:21]=1.C(Cl)(Cl)Cl>CN(C)C=O.O.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>[Cl:19][C:20]1[CH:25]=[CH:24][C:23]([C:2]2[CH:3]=[C:4]([C:8]([O:10][CH2:11][CH3:12])=[O:9])[N:5]([CH3:7])[CH:6]=2)=[C:22]([O:29][CH3:30])[CH:21]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 6212ChloroformHCID 10340Sodium CarbonateHCID 3858606(4-Chloro-2-methoxyphenyl)boronic acidHCID 72210990Ethyl 4-bromo-1-methyl-1H-pyrrole-2-carboxylate

生成物 1

HCID 86679343Ethyl 4-(4-chloro-2-methoxyphenyl)-1-methyl-1H-pyrrole-2-carboxylate収率 254.5%

試薬・触媒・溶媒 3

HCID 178418397
HCID 178418397、化合物
触媒
HCID 962Water溶媒2 回
HCID 6228Dimethylformamide溶媒

実験手順

Ethyl 4-bromo-1-methyl-1H-pyrrole-2-carboxylate (5.00 g, 21.6 mmol) prepared in the Step 10-1-2 was dissolved in N,N-dimethylformamide (20 ml)/water (5 ml), and sodium carbonate (6.87 g, 64.8 mmol), tetrakis(triphenylphosphine)palladium (120 mg, 0.1 mmol) and 4-chloro-2-methoxyphenylboronic acid (8.04 g, 4.32 mmol) was added to the solution. The mixture was heated under reflux for 5 hours. After the mixture was allowed to cool, water and chloroform was added to the mixture. The organic phase was collected by separation and dried over anhydrous magnesium sulfate. The solvent was distilled off, and the resulting residue was purified by silica gel column chromatography (ethyl acetate:n-hexane=1:3) to give the title compound (3.23 g, 51%).

後処理

  1. additionwas added to the solution
  2. temperatureThe mixture was heated
  3. temperatureunder reflux for 5 hours
  4. temperatureto cool
  5. customThe organic phase was collected by separation
  6. dry with materialdried over anhydrous magnesium sulfate
  7. distillationThe solvent was distilled off
  8. customthe resulting residue was purified by silica gel column chromatography (ethyl acetate:n-hexane=1:3)

出典と根拠

ORDレコード
ord-2ac76e0536ff4802825bc8e22b0e51ae
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09200008B2

反応ノート

読み込み中…

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