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Potassium Carbonate → Methyl 6-bromo-5-(2'-hydroxybiphenyl-4-yl)-1H-indole-3-carboxylate

HRID 338386
ノート
印刷プレビュー

反応式

HRID 338386 の反応式
[Br:1][C:2]1[CH:10]=[C:9]2[C:5]([C:6]([C:11]([O:13][CH3:14])=[O:12])=[CH:7][NH:8]2)=[CH:4][C:3]=1I.CC1(C)C(C)(C)OB([C:24]2[CH:29]=[CH:28][C:27]([C:30]3[C:31]([OH:36])=[CH:32][CH:33]=[CH:34][CH:35]=3)=[CH:26][CH:25]=2)O1.C(=O)([O-])[O-].[K+].[K+]>C1(C)C=CC=CC=1.C(O)C.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]>[Br:1][C:2]1[CH:10]=[C:9]2[C:5]([C:6]([C:11]([O:13][CH3:14])=[O:12])=[CH:7][NH:8]2)=[CH:4][C:3]=1[C:24]1[CH:25]=[CH:26][C:27]([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=2[OH:36])=[CH:28][CH:29]=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 11430Potassium CarbonateHCID 592678134'-(4,4,5,5-Tetramethyl-1,3,2-dioxaborolan-2-yl)-[1,1'-biphenyl]-2-olHCID 86698727methyl 6-bromo-5-iodo-1H-indole-3-carboxylate

生成物 1

HCID 86698726Methyl 6-bromo-5-(2'-hydroxybiphenyl-4-yl)-1H-indole-3-carboxylate

試薬・触媒・溶媒 3

HCID 44119782
Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)
触媒
HCID 702Ethanol溶媒
HCID 1140Toluene溶媒

反応条件

温度
110 °C

実験手順

To a solution of methyl 6-bromo-5-iodo-1H-indole-3-carboxylate (100 mg, 0.26 mmol) in toluene (1 ml) and ethanol (1 ml) was added 4′-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)biphenyl-2-ol (70 mg, 0.24 mmol) followed by aqueous potassium carbonate (2M, 1 ml, 2.0 mmol). The solvent was degassed by passing nitrogen through the system for 5 min. Pd(dppf)Cl2 (10 mg, 0.0053 mmol) was added then sealed and reaction heated to 110° C. The reaction was cooled then partitioned between water and ethyl acetate, then washed with brine, dried over sodium sulfate, filtered, concentrated in vacuo to afford the title compound mixed with unidentified byproducts as a dark tan solid (120 mg). TLC (50% EtOAc/Heptane) indicates no separation between product and byproducts. Crude was taken on to the next step without purification.

後処理

  1. customThe solvent was degassed
  2. customfor 5 min
  3. customthen sealed
  4. customreaction
  5. temperatureThe reaction was cooled
  6. customthen partitioned between water and ethyl acetate
  7. washwashed with brine
  8. dry with materialdried over sodium sulfate
  9. filtrationfiltered
  10. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-9eb44053fe3240b0ba4864908a5ed2fe
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08889730B2

反応ノート

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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