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Sodium Carbonate → 6-(5-(Methylthio)-1,3,4-thiadiazol-2-yl)isoquinoline

HRID 2075364
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인쇄 미리보기

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HRID 2075364 반응식
Br[C:2]1[S:3][C:4]([S:7][CH3:8])=[N:5][N:6]=1.[CH:9]1[C:18]2[C:13](=[CH:14][C:15](B(O)O)=[CH:16][CH:17]=2)[CH:12]=[CH:11][N:10]=1.C([O-])([O-])=O.[Na+].[Na+]>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.COCCOC>[CH3:8][S:7][C:4]1[S:3][C:2]([C:15]2[CH:14]=[C:13]3[C:18](=[CH:17][CH:16]=2)[CH:9]=[N:10][CH:11]=[CH:12]3)=[N:6][N:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 10340Sodium CarbonateHCID 222696212-Bromo-5-(methylsulfanyl)-1,3,4-thiadiazoleHCID 44119669(Isoquinolin-6-yl)boronic acid

생성물 1

HCID 579918536-(5-(Methylthio)-1,3,4-thiadiazol-2-yl)isoquinoline수율 59%

시약·촉매·용매 2

HCID 178418397HCID 178418397, 화합물촉매
HCID 8071
1,2-Dimethoxyethane
용매

실험 절차

To a 25 mL round bottom flask was added 2-bromo-5-(methylthio)-1,3,4-thiadiazole (0.40 g, 1.9 mmol) (prepared as described in WO 97/30981, isoquinolin-6-ylboronic acid (0.39 g, 2.3 mmol) (prepared as described in US Patent Publication No. US 2007/0173506), Pd(PPh3)4 (0.11 g, 0.095 mmol), 2.4 mL of a 2 M Na2CO3 aqueous solution and 2 mL of DME. The reaction was heated at reflux for 16 hours. The reaction mixture was concentrated, and the residue was purified by column chromatography on silica gel (eluting with a gradient from 0 to 70% EtOAc in hexanes) to provide 6-(5-(methylthio)-1,3,4-thiadiazol-2-yl)isoquinoline (0.29 g, 59%) as a yellow solid. LCMS (M+H) 260 calc. for C12H10N3S2 260.0.

후처리

  1. customprepared
  2. temperatureThe reaction was heated
  3. temperatureat reflux for 16 hours
  4. concentrationThe reaction mixture was concentrated
  5. customthe residue was purified by column chromatography on silica gel (
  6. washeluting with a gradient from 0 to 70% EtOAc in hexanes)

출처 및 근거

ORD 기록
ord-b7cc061bbd72486096460119576935b8
출처 데이터셋
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07919504B2

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