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Potassium Carbonate → HCID 58229488、化合物

HRID 1963776
ノート
印刷プレビュー

反応式

HRID 1963776 の反応式
[Cl:1][C:2]1[C:7]([NH:8][S:9]([C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=2)(=[O:11])=[O:10])=[CH:6][C:5](B2OC(C)(C)C(C)(C)O2)=[CH:4][N:3]=1.Br[C:29]1[CH:30]=[C:31]2[C:36](=[CH:37][CH:38]=1)[N:35]=[CH:34][C:33]([OH:39])=[CH:32]2.C(=O)([O-])[O-].[K+].[K+]>O1CCOCC1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2].C(Cl)Cl>[Cl:1][C:2]1[C:7]([NH:8][S:9]([C:12]2[CH:13]=[CH:14][C:15]([F:18])=[CH:16][CH:17]=2)(=[O:10])=[O:11])=[CH:6][C:5]([C:29]2[CH:30]=[C:31]3[C:36](=[CH:37][CH:38]=2)[N:35]=[CH:34][C:33]([OH:39])=[CH:32]3)=[CH:4][N:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 170396516-Bromoquinolin-3-olHCID 53363355n-[2-Chloro-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridin-3-yl]-4-fluorobenzene-1-sulfonamide

生成物 1

HCID 58229488HCID 58229488、化合物収率 63.1%

試薬・触媒・溶媒 2

HCID 178418807HCID 178418807、化合物触媒
HCID 312751,4-Dioxane溶媒

実験手順

To a microwave vial (5 mL) was added N-(2-chloro-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridin-3-yl)-4-fluorobenzenesulfonamide (0.129 g, 0.312 mmol), 6-bromoquinolin-3-ol (Li et. Al, Bioorganic & Medicinal Chemistry Letters (2006), 16(7), 2000-2007) (0.0703 g, 0.314 mmol), PdCl2(dppf)-CH2Cl2 adduct (0.0128 g, 0.0156 mmol) and potassium carbonate (2.0 M, 0.390 mL, 0.781 mmol) in 1,4-dioxane (3 mL). The mixture was degassed by bubbling nitrogen through for 10 min. The tube was irradiated with microwave at 100° C. for 10 min. The reaction mixture was cooled to RT then partitioned between water (10 mL) and EtOAc (10 mL). The product went into aqueous almost exclusively. The aqueous phase was passed through BE-SCX column (Varian, Palo Alto, Calif., 10 gm) then eluted with MeOH. MeOH fraction contains the product. MeOH was evaporated and yielded a brown solid (0.0846 g) as the desired product. m/z: calc'd for C20H13ClFN3O3S: 429.0; found 430.0 (M+1). 1H NMR (300 MHz, DMSO-d6) δ ppm 7.21-7.35 (m, 2 H), 7.52-7.65 (m, 2 H), 7.74-7.86 (m, 3 H), 7.89 (d, J=1.8 Hz, 1 H), 7.96 (d, J=8.6 Hz, 1 H), 8.03-8.15 (m, 1 H), 8.58 (d, J=2.8 Hz, 1 H), 10.40 (s, 1 H).

後処理

  1. customThe mixture was degassed
  2. customby bubbling nitrogen through for 10 min
  3. customThe tube was irradiated with microwave at 100° C. for 10 min
  4. customthen partitioned between water (10 mL) and EtOAc (10 mL)
  5. washthen eluted with MeOH
  6. customMeOH was evaporated

出典と根拠

ORDレコード
ord-53ab902836fe4d4c86cd143d1bf9ca6b
出典データセット
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08415376B2

反応ノート

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