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Toluene → HCID 67354151、化合物

HRID 2272278
ノート
印刷プレビュー

反応式

HRID 2272278 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[O:9][C:10]3[CH:19]=[C:18]([N+:20]([O-:22])=[O:21])[C:17](OS(C(F)(F)F)(=O)=O)=[CH:16][C:11]=3[C:12]=2[C:13]([O-:15])=[O:14])=[CH:4][CH:3]=1.[F-].[K+].[Na+].[Br-].[CH:35]1(B(O)O)[CH2:37][CH2:36]1.[C:41]1(C)C=CC=C[CH:42]=1>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.O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[O:9][C:10]3[CH:19]=[C:18]([N+:20]([O-:22])=[O:21])[C:17]([CH:35]4[CH2:37][CH2:36]4)=[CH:16][C:11]=3[C:12]=2[C:13]([O:15][CH2:41][CH3:42])=[O:14])=[CH:6][CH:7]=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 5

HCID 1140TolueneHCID 253881Sodium BromideHCID 522689Potassium FluorideHCID 2760897Cyclopropylboronic acidHCID 86696005HCID 86696005、化合物

生成物 1

HCID 67354151HCID 67354151、化合物収率 99%

試薬・触媒・溶媒 2

HCID 178418397
HCID 178418397、化合物
触媒
HCID 962Water溶媒

実験手順

A mixture of 2-(4-chlorophenyl)-6-nitro-5-(trifluoromethylsulfonyloxy)benzofuran-3-carboxylate (10 g, 18 mmol), KF (4.64 g, 79.9 mmol), NaBr (2.48 g, 24 mmol), cyclopropylboronic acid (3.2 g, 37 mmol), and Pd(Ph3P)4 (1.33 g, 1.15 mmol) were added toluene (130 mL) and water (2.8 mL). The reaction flask was evacuated for ˜3 minutes then filled with nitrogen. The reaction mixture was refluxed under nitrogen for 20 hrs then cooled to ambient temperature. The reaction mixture was diluted with EtOAc (150 mL), washed with water (3×200 mL), brine (200 mL), dried with anhydrous sodium sulfate, decanted, and concentrated under reduced pressure. The residue was purified by column chromatography (petroleum ether/ethyl acetate=30/1-10/1) to afford ethyl 2-(4-chlorophenyl)-5-cyclopropyl-6-nitrobenzofuran-3-carboxylate as a yellow solid (7.9 g, 99%).

後処理

  1. customThe reaction flask was evacuated for ˜3 minutes
  2. additionthen filled with nitrogen
  3. temperatureThe reaction mixture was refluxed under nitrogen for 20 hrs
  4. additionThe reaction mixture was diluted with EtOAc (150 mL)
  5. washwashed with water (3×200 mL), brine (200 mL)
  6. dry with materialdried with anhydrous sodium sulfate
  7. customdecanted
  8. concentrationconcentrated under reduced pressure
  9. customThe residue was purified by column chromatography (petroleum ether/ethyl acetate=30/1-10/1)

出典と根拠

ORDレコード
ord-16a1c65cfafe4ac8a910e6428939707e
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09119868B2

反応ノート

読み込み中…

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