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Cesium carbonate → 6-Chloro-4'-(ethylsulfonyl)-2'-methoxy-[1,1'-biphenyl]-3-ol

HRID 1846034
ノート
印刷プレビュー

反応式

HRID 1846034 の反応式
C([Si]([O:8][C:9]1[CH:14]=[CH:13][C:12]([Cl:15])=[C:11](I)[CH:10]=1)(C)C)(C)(C)C.[CH2:17]([S:19]([C:22]1[CH:27]=[CH:26][C:25](B2OC(C)(C)C(C)(C)O2)=[C:24]([O:37][CH3:38])[CH:23]=1)(=[O:21])=[O:20])[CH3:18].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]>[Cl:15][C:12]1[C:11]([C:25]2[CH:26]=[CH:27][C:22]([S:19]([CH2:17][CH3:18])(=[O:21])=[O:20])=[CH:23][C:24]=2[O:37][CH3:38])=[CH:10][C:9]([OH:8])=[CH:14][CH:13]=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 867232082-(4-(Ethylsulfonyl)-2-methoxyphenyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolaneHCID 86723256tert-Butyl(4-chloro-3-iodophenoxy)dimethylsilane

生成物 1

HCID 867232576-Chloro-4'-(ethylsulfonyl)-2'-methoxy-[1,1'-biphenyl]-3-ol収率 72%

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
100 °C

実験手順

A solution of tert-butyl(4-chloro-3-iodophenoxy)dimethylsilane (Preparation 53, 102 mg, 0.28 mmol), 2-(4-(ethylsulfonyl)-2-methoxyphenyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (Preparation 21) (90 mg, 0.28 mmol) and aqueous caesium carbonate solution (1M, 0.55 mL, 0.55 mmol) in dioxane (4 mL) was degassed with nitrogen for 10 minutes, followed by the addition of 1,1′-bis(diphenylphosphino)ferrocene-palladium(II)dichloride (11.0 mg, 0.014 mmol). The resulting mixture was heated at 100° C. for 3 hours and then cooled to room temperature. The mixture was partitioned between water (15 mL) and EtOAc (15 mL), the aqueous layer then extracted with EtOAc (2×15 mL). The organic layers were combined and washed with brine (25 mL), dried over MgSO4 and then concentrated in vacuo. 4M HCl in dioxane (4 mL) was added to the residue, and the mixture stirred at room temperature for 40 hours. After concentration in vacuo, NH3 solution (7M in MeOH, 2 mL) was added to the residue, and the mixture re-concentrated in vacuo. The residue was purified by silica gel column chromatography eluting with cyclohexane/EtOAc 70:30 to afford the title compound as yellow gum in 72% yield, 65 mg.

後処理

  1. temperaturecooled to room temperature
  2. customThe mixture was partitioned between water (15 mL) and EtOAc (15 mL)
  3. extractionthe aqueous layer then extracted with EtOAc (2×15 mL)
  4. washwashed with brine (25 mL)
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated in vacuo
  7. addition4M HCl in dioxane (4 mL) was added to the residue
  8. concentrationAfter concentration in vacuo, NH3 solution (7M in MeOH, 2 mL)
  9. additionwas added to the residue
  10. concentrationthe mixture re-concentrated in vacuo
  11. customThe residue was purified by silica gel column chromatography
  12. washeluting with cyclohexane/EtOAc 70:30

出典と根拠

ORDレコード
ord-3ea84e7ee23444199c742995855f39ce
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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