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Toluene → HCID 67354151, 화합물

HRID 2272278
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HRID 2272278 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 1140TolueneHCID 253881Sodium BromideHCID 522689Potassium FluorideHCID 2760897Cyclopropylboronic acidHCID 86696005HCID 86696005, 화합물

생성물 1

HCID 67354151HCID 67354151, 화합물수율 99%

시약·촉매·용매 2

HCID 178418397
HCID 178418397, 화합물
촉매
HCID 962Water용매

실험 절차

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%).

후처리

  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)

출처 및 근거

ORD 기록
ord-16a1c65cfafe4ac8a910e6428939707e
출처 데이터셋
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09119868B2

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