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

Sodium Carbonate → 2'-Fluoro-5'-(7-isopropyl-7H-imidazo[4,5-c]pyridazin-4-yl)biphenyl-4-sulfonamide

HRID 1845988
ノート
印刷プレビュー

反応式

HRID 1845988 の反応式
Cl[C:2]1[C:3]2[N:10]=[CH:9][N:8]([CH:11]([CH3:13])[CH3:12])[C:4]=2[N:5]=[N:6][CH:7]=1.[F:14][C:15]1[CH:20]=[CH:19][C:18](B2OC(C)(C)C(C)(C)O2)=[CH:17][C:16]=1[C:30]1[CH:35]=[CH:34][C:33]([S:36]([NH2:39])(=[O:38])=[O:37])=[CH:32][CH:31]=1.C([O-])([O-])=O.[Na+].[Na+]>O1CCOCC1.O.C1C=CC(P([C]2[CH][CH][CH][CH]2)C2C=CC=CC=2)=CC=1.C1C=CC(P([C]2[CH][CH][CH][CH]2)C2C=CC=CC=2)=CC=1.Cl[Pd]Cl.[Fe]>[F:14][C:15]1[CH:20]=[CH:19][C:18]([C:2]2[C:3]3[N:10]=[CH:9][N:8]([CH:11]([CH3:13])[CH3:12])[C:4]=3[N:5]=[N:6][CH:7]=2)=[CH:17][C:16]=1[C:30]1[CH:35]=[CH:34][C:33]([S:36]([NH2:39])(=[O:37])=[O:38])=[CH:32][CH:31]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 10340Sodium CarbonateHCID 867232144-chloro-7-isopropyl-7H-imidazo[4,5-c]pyridazineHCID 867232162'-Fluoro-5'-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-[1,1'-biphenyl]-4-sulfonamide

生成物 1

HCID 867232152'-Fluoro-5'-(7-isopropyl-7H-imidazo[4,5-c]pyridazin-4-yl)biphenyl-4-sulfonamide収率 50%

試薬・触媒・溶媒 3

HCID 178477754
HCID 178477754、化合物
触媒
HCID 962Water溶媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
90 °C

実験手順

To 4-Chloro-7-isopropyl-7H-imidazo[4,5-c]pyridazine (Preparation 6, 50 mg, 0.254 mmoles) and 2′-fluoro-5′-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)biphenyl-4-sulfonamide (Preparation 2, 131 mg, 0.254 mmoles) in dioxane (2.5 mL) was added Na2CO3 (80 mg, 0.759 mmol) pre dissolved in water (0.5 mL) and [1,1-bis(diphenylphosphino)ferrocene]dichloropalladium(II) (7.3 mg, 0.009 mmol). The reaction was degassed with nitrogen and heated under microwave irradiation at 90° C. for 15 minutes. After cooling, ethyl acetate and Na2SO4 were added and the mixture decanted and washed with ethyl acetate. Purification by silica gel column chromatography eluting with DCM: MeOH 1:0 to 9:1 yielded the title product in 50% yield, 57 mg.

後処理

  1. customThe reaction was degassed with nitrogen
  2. temperatureAfter cooling
  3. additionethyl acetate and Na2SO4 were added
  4. customthe mixture decanted
  5. washwashed with ethyl acetate
  6. customPurification by silica gel column chromatography
  7. washeluting with DCM: MeOH 1:0 to 9:1

出典と根拠

ORDレコード
ord-19451d24ac21407fb72bead5df319d90
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08952008B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート