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Cesium carbonate → 5'-Bromo-4-(ethylsulfonyl)-2,2'-dimethoxy-1,1-biphenyl

HRID 1846036
ノート
印刷プレビュー

反応式

HRID 1846036 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[C:4](I)[CH:3]=1.[CH2:11]([S:13]([C:16]1[CH:21]=[CH:20][C:19](B2OC(C)(C)C(C)(C)O2)=[C:18]([O:31][CH3:32])[CH:17]=1)(=[O:15])=[O:14])[CH3:12].C(=O)([O-])[O-].[Cs+].[Cs+]>O1CCOCC1.[Pd](Cl)Cl.C1(P(C2C=CC=CC=2)[C-]2C=CC=C2)C=CC=CC=1.[C-]1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=C1.[Fe+2]>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[C:4]([C:19]2[CH:20]=[CH:21][C:16]([S:13]([CH2:11][CH3:12])(=[O:15])=[O:14])=[CH:17][C:18]=2[O:31][CH3:32])[CH:3]=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

6

反応物 3

HCID 10796Cesium carbonateHCID 109799044-Bromo-2-iodo-1-methoxybenzeneHCID 867232082-(4-(Ethylsulfonyl)-2-methoxyphenyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane

生成物 1

HCID 867232595'-Bromo-4-(ethylsulfonyl)-2,2'-dimethoxy-1,1-biphenyl収率 45%

試薬・触媒・溶媒 2

HCID 44119782
Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)
触媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
80 °C

実験手順

A solution of 4-bromo-2-iodo-1-methoxybenzene (Preparation 57, 350 mg, 1.12 mmol), 2-(4-(ethylsulfonyl)-2-methoxyphenyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (Preparation 21, 365 mg, 1.12 mmol) and aqueous caesium carbonate solution (1M, 2.23 mL, 2.23 mmol) in dioxane (18 mL) was degassed with nitrogen for 10 min, followed by addition of 1,1′-bis(diphenylphosphino)ferrocene-palladium(II)dichloride (46.0 mg, 0.0056 mmol). The resulting mixture was heated at 80° C. for 16 hours. After cooling to room temperature and concentration in vacuo, the crude residue was partitioned between water (30 mL) and EtOAc (30 mL). The aqueous layer was extracted with EtOAc (2×20 mL). The organic layers were combined and washed with brine (25 mL), dried over MgSO4 and concentrated in vacuo. The residue was purified by silica gel column chromatography eluting with heptanes/EtOAc (70:30), to afford the title compound as off-white solid in 45% yield, 150 mg.

後処理

  1. temperatureAfter cooling to room temperature
  2. concentrationconcentration in vacuo
  3. customthe crude residue was partitioned between water (30 mL) and EtOAc (30 mL)
  4. extractionThe aqueous layer was extracted with EtOAc (2×20 mL)
  5. washwashed with brine (25 mL)
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated in vacuo
  8. customThe residue was purified by silica gel column chromatography
  9. washeluting with heptanes/EtOAc (70:30)

出典と根拠

ORDレコード
ord-0e5d24f2ee2444a9a172268d609a667d
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

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