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Dichloromethane → N-tert-Butyl-3'-fluoro-4'-quinoxalin-6-ylbiphenyl-2-sulfonamide

HRID 1523943
ノート
印刷プレビュー

反応式

HRID 1523943 の反応式
Br[C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:9]([S:14]([NH:17][C:18]([CH3:21])([CH3:20])[CH3:19])(=[O:16])=[O:15])=[CH:10][CH:11]=[CH:12][CH:13]=2)=[CH:4][C:3]=1[F:22].CC1(C)C(C)(C)OB([C:31]2[CH:32]=[C:33]3[C:38](=[CH:39][CH:40]=2)[N:37]=[CH:36][CH:35]=[N:34]3)O1.C([O-])([O-])=O.[Na+].[Na+].C(Cl)Cl>C(OCC)(=O)C.O.O1CCOCC1>[C:18]([NH:17][S:14]([C:9]1[C:8]([C:5]2[CH:6]=[CH:7][C:2]([C:31]3[CH:32]=[C:33]4[C:38](=[CH:39][CH:40]=3)[N:37]=[CH:36][CH:35]=[N:34]4)=[C:3]([F:22])[CH:4]=2)=[CH:13][CH:12]=[CH:11][CH:10]=1)(=[O:16])=[O:15])([CH3:21])([CH3:20])[CH3:19]
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

8

反応物 4

HCID 6344DichloromethaneHCID 10340Sodium CarbonateHCID 441182986-(4,4,5,5-Tetramethyl-1,3,2-dioxaborolan-2-yl)quinoxalineHCID 903130764'-Bromo-N-(tert-butyl)-3'-fluoro-[1,1'-biphenyl]-2-sulfonamide

生成物 1

HCID 90313194N-tert-Butyl-3'-fluoro-4'-quinoxalin-6-ylbiphenyl-2-sulfonamide

試薬・触媒・溶媒 3

HCID 962
Water
溶媒
HCID 8857Ethyl Acetate溶媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
80 °C

実験手順

4′-Bromo-N-(tert-butyl)-3′-fluoro-[1,1′-biphenyl]-2-sulfonamide (30 mg, 0.078 mmol) and 6-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)quinoxaline (12 mg, 0.085 mmol) were added to a 5 mL sealable vial equipped with a stir bar. Dioxane (0.2 mL) and 2 M Na2CO3 (0.2 mL) were added. Argon was bubbled through the solvent while it was rapidly stirred for 10 min then Pd(dppf)Cl2.CH2Cl2 (3 mg, 0.004 mmol) was added, and the mixture heated for 15 hours at 80° Celsius under an argon atmosphere. The reaction was diluted with 2 mL of ethyl acetate and 2 mL of water and the aqueous layer was extracted with ethyl acetate (3×10 mL). The combined organic extracts were then dried with Na2SO4 and concentrated to dryness. The crude product was purified by HPLC to give the title compound. MS (ESI): mass calcd. for C24H22FN3O2S, 435.14; m/z found, 436.4 [M+H]+. 1H NMR (500 MHz, CDCl3) δ 8.93-8.91 (d, J=1.8, 1H), 8.91-8.89 (d, J=1.8, 1H), 8.37-8.34 (m, 1H), 8.24-8.22 (m, 1H), 8.22-8.20 (m, 1H), 8.09-8.04 (m, 1H), 7.71-7.66 (m, 1H), 7.65-7.59 (m, 1H), 7.58-7.52 (m, 1H), 7.51-7.44 (dd, J=7.9, 1.8, 1H), 7.44-7.40 (dd, J=11.3, 1.7, 1H), 7.40-7.36 (dd, J=7.5, 1.4, 1H), 3.74 (s, 1H), 1.10 (s, 9H).

後処理

  1. customequipped with a stir bar
  2. customArgon was bubbled through the solvent while it
  3. extractionthe aqueous layer was extracted with ethyl acetate (3×10 mL)
  4. dry with materialThe combined organic extracts were then dried with Na2SO4
  5. concentrationconcentrated to dryness
  6. customThe crude product was purified by HPLC

出典と根拠

ORDレコード
ord-52382f87834f48cfa03c3c0218e60069
出典データセット
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09079866B2

反応ノート

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