홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Potassium Carbonate → 1-(3'-fluoro-[1,1'-biphenyl]-4-yl)-N-(pyrimidin-4-yl)isoquinoline-6-sulfonamide

HRID 1473611
노트
인쇄 미리보기

반응식

HRID 1473611 반응식
Cl[C:2]1[C:11]2[C:6](=[CH:7][C:8]([S:12]([NH:15][C:16]3[CH:21]=[CH:20][N:19]=[CH:18][N:17]=3)(=[O:14])=[O:13])=[CH:9][CH:10]=2)[CH:5]=[CH:4][N:3]=1.Cl[C:23]1[CH:28]=[CH:27][C:26](B(O)O)=[CH:25][CH:24]=1.C(=O)([O-])[O-].[K+].[K+].[F:38][C:39]1[CH:40]=[C:41](B(O)O)[CH:42]=[CH:43][CH:44]=1.C1(P(C2CCCCC2)C2C=CC=CC=2C2C(OC)=CC=CC=2OC)CCCCC1>C(OCC)(=O)C.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>[F:38][C:39]1[CH:40]=[C:41]([C:23]2[CH:28]=[CH:27][C:26]([C:2]3[C:11]4[C:6](=[CH:7][C:8]([S:12]([NH:15][C:16]5[CH:21]=[CH:20][N:19]=[CH:18][N:17]=5)(=[O:14])=[O:13])=[CH:9][CH:10]=4)[CH:5]=[CH:4][N:3]=3)=[CH:25][CH:24]=2)[CH:42]=[CH:43][CH:44]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 11430Potassium CarbonateHCID 742994-Chlorophenylboronic acidHCID 27339863-Fluorophenylboronic acidHCID 112698722-Dicyclohexylphosphino-2',6'-dimethoxybiphenylHCID 866876591-chloro-N-(pyrimidin-4-yl)isoquinoline-6-sulfonamide

생성물 1

HCID 86687676
1-(3'-fluoro-[1,1'-biphenyl]-4-yl)-N-(pyrimidin-4-yl)isoquinoline-6-sulfonamide

시약·촉매·용매 2

HCID 178418397HCID 178418397, 화합물촉매HCID 8857Ethyl Acetate용매

실험 절차

A vial was charged with 1-chloro-N-(pyrimidin-4-yl)isoquinoline-6-sulfonamide (0.075 g, 0.234 mmol), (4-chlorophenyl)boronic acid (0.040 g, 0.257 mmol), Pd(Ph3P)4 (0.027 g, 0.023 mmol), and potassium carbonate (0.097 g, 0.701 mmol). The vial was flushed with Ar (g), then 1,4-dioxane (0.877 ml) and Water (0.292 ml) were added in sequence. The vial was sealed and microwaved at 100° C. for 30 minutes. (3-fluorophenyl)boronic acid (0.065 g, 0.468 mmol), dicyclohexyl(2′,6′-dimethoxy-[1,1′-biphenyl]-2-yl)phosphine (4.80 mg, 0.012 mmol), and chloro(2-dicyclohexylphosphino-2′,6′-dimethoxy-1,1′-biphenyl)[2-(2-aminoethylphenyl)]palladium(ii) dichloromethane (8.86 mg, 0.012 mmol) were added and the reaction was microwaved at 100° C. for 45 minutes. The reaction was diluted with ethyl acetate and washed with water. The aqueous layer was extracted with ethyl acetate, and the combined organic layers were dried with sodium sulfate, filtered, and concentrated. The material was purified via column chromatography (RediSep Gold 12 g, gradient elution 0-10% MeOH:DCM) to afford 1-(3′-fluoro-[1,1′-biphenyl]-4-yl)-N-(pyrimidin-4-yl)isoquinoline-6-sulfonamide as a light yellow solid. 1H NMR (400 MHz, DMSO-d6) δ=8.74 (d, J=5.8 Hz, 1H), 8.70 (br. s., 1H), 8.58 (br. s., 1H), 8.23 (d, J=9.1 Hz, 2H), 8.13 (d, J=5.5 Hz, 1H), 8.03 (d, J=9.3 Hz, 1H), 7.92 (d, J=8.3 Hz, 2H), 7.80 (d, J=8.2 Hz, 2H), 7.66 (d, J=8.0 Hz, 2H), 7.60-7.51 (m, 2H), 7.30-7.20 (m, 2H), 7.15-6.97 (m, 1H). m/z (ESI) 457.2 (M+H)+.

후처리

  1. customThe vial was flushed with Ar (g)
  2. addition1,4-dioxane (0.877 ml) and Water (0.292 ml) were added in sequence
  3. customThe vial was sealed
  4. custommicrowaved at 100° C. for 30 minutes
  5. customthe reaction was microwaved at 100° C. for 45 minutes
  6. washwashed with water
  7. extractionThe aqueous layer was extracted with ethyl acetate
  8. dry with materialthe combined organic layers were dried with sodium sulfate
  9. filtrationfiltered
  10. concentrationconcentrated
  11. customThe material was purified via column chromatography (RediSep Gold 12 g, gradient elution 0-10% MeOH:DCM)

출처 및 근거

ORD 기록
ord-4e8dfd23990f42ee8d445d1d9cc3137f
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09012443B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트