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Potassium Phosphate, Tribasic → HCID 86701700、化合物

HRID 2174069
ノート
印刷プレビュー

反応式

HRID 2174069 の反応式
Br[C:2]1[C:10]2[C:9]([CH:11]=[O:12])=[C:8]([CH3:13])[CH:7]=[C:6]([CH3:14])[C:5]=2[N:4]([S:15]([C:18]2[CH:24]=[CH:23][C:21]([CH3:22])=[CH:20][CH:19]=2)(=[O:17])=[O:16])[CH:3]=1.[C:25]1(B(O)O)[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1.[O-]P([O-])([O-])=O.[K+].[K+].[K+].COC1C=CC=C(OC)C=1C1C=CC=CC=1P(C1CCCCC1)C1CCCCC1>COCCOC.C(Cl)Cl.O.CC([O-])=O.CC([O-])=O.[Pd+2]>[CH3:13][C:8]1[CH:7]=[C:6]([CH3:14])[C:5]2[N:4]([S:15]([C:18]3[CH:24]=[CH:23][C:21]([CH3:22])=[CH:20][CH:19]=3)(=[O:16])=[O:17])[CH:3]=[C:2]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)[C:10]=2[C:9]=1[CH:11]=[O:12]
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

9

反応物 4

HCID 62657Potassium Phosphate, TribasicHCID 66827Phenylboronic AcidHCID 112698722-Dicyclohexylphosphino-2',6'-dimethoxybiphenylHCID 867016993-Bromo-5,7-dimethyl-1-tosyl-1H-indole-4-carbaldehyde

生成物 1

HCID 86701700HCID 86701700、化合物

試薬・触媒・溶媒 4

HCID 167845
palladium(II) acetate
触媒
HCID 962Water溶媒2 回
HCID 6344Dichloromethane溶媒
HCID 80711,2-Dimethoxyethane溶媒

反応条件

温度
80 °C

実験手順

To a suspension of 3-bromo-5,7-dimethyl-1-tosyl-1H-indole-4-carbaldehyde (100 mg, 0.246 mmol), phenylboronic acid (60.0 mg, 0.492 mmol), and K3PO4 (157 mg, 0.738 mmol) in DME (1 mL)/H2O (0.5 mL), Pd(OAc)2 (5.53 mg, 0.025 mmol) and S-phos (CAS#657408-07-6) (20.21 mg, 0.049 mmol) were added the mixture was stirred at 80° C. for 15 h. The reaction mixture was cooled to room temperature and diluted with CH2Cl2 and water. The layers were partitioned. The organic layer was separated, dried over MgSO4, filtered and concentrated. The resulting residue was purified by silica gel flash column chromatography [heptane/(30% EtOAc in CH2Cl2)=1/0 to 4/6] to give the title compound. MS (ESI+) m/z 404.1 (M+H).

後処理

  1. additionwere added the mixture
  2. temperatureThe reaction mixture was cooled to room temperature
  3. customThe layers were partitioned
  4. customThe organic layer was separated
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe resulting residue was purified by silica gel flash column chromatography [heptane/(30% EtOAc in CH2Cl2)=1/0 to 4/6]

出典と根拠

ORDレコード
ord-43178539b2e6408694bd073248fa5859
出典データセット
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09056874B2

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