ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

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

HRID 1473611
ノート
印刷プレビュー

反応式

HRID 1473611 の反応式
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
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 11430Potassium CarbonateHCID 742994-Chlorophenylboronic acidHCID 27339863-Fluorophenylboronic acidHCID 112698722-Dicyclohexylphosphino-2',6'-dimethoxybiphenylHCID 866876591-chloro-N-(pyrimidin-4-yl)isoquinoline-6-sulfonamide

生成物 1

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

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒HCID 8857Ethyl Acetate溶媒

実験手順

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)+.

後処理

  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)

出典と根拠

ORDレコード
ord-4e8dfd23990f42ee8d445d1d9cc3137f
出典データセット
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09012443B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート