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Potassium Carbonate → 2,6-Dimethylisoquinolin-1-one

HRID 518296
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HRID 518296 반응식
Br[C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[C:8](=[O:12])[N:7]([CH3:13])[CH:6]=[CH:5]2.[CH3:14]B(O)O.C([O-])([O-])=O.[K+].[K+]>O.O1CCOCC1.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>[CH3:13][N:7]1[CH:6]=[CH:5][C:4]2[C:9](=[CH:10][CH:11]=[C:2]([CH3:14])[CH:3]=2)[C:8]1=[O:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 11430Potassium CarbonateHCID 139377Methylboronic AcidHCID 231581786-Bromo-2-methyl-1,2-dihydroisoquinolin-1-one

생성물 1

HCID 140926042,6-Dimethylisoquinolin-1-one수율 82.8%

시약·촉매·용매 3

HCID 962Water촉매
HCID 178418397
HCID 178418397, 화합물
촉매
HCID 312751,4-Dioxane용매

실험 절차

A mixture of 6-bromo-2-methylisoquinolin-1-one (200.0 mg, 0.84 mmol), methylboronic acid (251.0 mg, 4.2 mmol), Pd(PPh3)4 (93.0 mg, 0.08 mmol), K2CO3 (232.0 mg, 1.68 mmol) and H2O (2 drops) in dioxane (10.0 mL) was microwaved at 120° C. for 1 h. Purification by silica gel chromatography (PE:EA=5:1) gave the title compound (120.0 mg, 82.8%) as a light yellow solid. LCMS: 174.3 (M+H)+.

후처리

  1. customwas microwaved at 120° C. for 1 h
  2. customPurification by silica gel chromatography (PE:EA=5:1)

출처 및 근거

ORD 기록
ord-ea6d06431c684feaa1c8ef0114597e06
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09115114B2

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