Potassium Phosphate, Tribasic → HCID 70202778、化合物

HRID 2367930ノート

反応式

HRID 2367930 の反応式
[CH3:1][O:2][C:3]1[CH:19]=[CH:18][C:6]([CH2:7][O:8][C:9]2[CH:10]=[C:11](B(O)O)[CH:12]=[CH:13][CH:14]=2)=[CH:5][CH:4]=1.Br[C:21]1[S:22][CH:23]=[C:24]([C:26]([O:28][CH3:29])=[O:27])[N:25]=1.C1(P(C2CCCCC2)C2C=CC=CC=2C2C(OC)=CC=CC=2OC)CCCCC1.[O-]P([O-])([O-])=O.[K+].[K+].[K+]>C1(C)C=CC=CC=1.O.C(OCC)(=O)C.Cl[Pd]Cl>[CH3:1][O:2][C:3]1[CH:19]=[CH:18][C:6]([CH2:7][O:8][C:9]2[CH:10]=[C:11]([C:21]3[S:22][CH:23]=[C:24]([C:26]([O:28][CH3:29])=[O:27])[N:25]=3)[CH:12]=[CH:13][CH:14]=2)=[CH:5][CH:4]=1

参加物

9

反応物 4

HCID 62657Potassium Phosphate, TribasicHCID 2763213Methyl 2-bromothiazole-4-carboxylateHCID 112698722-Dicyclohexylphosphino-2',6'-dimethoxybiphenylHCID 16218173{3-[(4-Methoxyphenyl)methoxy]phenyl}boronic acid

生成物 1

HCID 70202778HCID 70202778、化合物

試薬・触媒・溶媒 4

HCID 24290Palladium Chloride触媒HCID 962Water溶媒HCID 1140Toluene溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
180 °C

実験手順

3-(4-methoxybenzyloxy)phenylboronic acid (697 mg, 2.7 mmol, 1.5 eq.), methyl 2-bromothiazole-4-carboxylate (400 mg, 1.8 mmol, 1.0 eq.), dicyclohexyl (2′,6′-dimethoxybiphenyl-2-yl) phosphine (74 mg, 0.18 mmol, 10 mol %) and PdCl2 (20 mg, 0.090 mmol, 5 mol %) were dissolved in toluene (6 mL) and added to a solution of K3PO4 (828 mg, 3.6 mmol, 2.0 eq.) in water (0.6 mL). The reaction mixture was heated 20 min at 180° C. in a microwave reactor, allowed to cool, diluted with ethyl acetate, washed with brine, dried over anhydrous sodium sulfate and concentrated in vacuo. The crude 23 was used in the next step without purification.

後処理

  1. temperatureto cool
  2. washwashed with brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe crude 23 was used in the next step without purification

出典と根拠

ORDレコード
ord-401dcfef1b1f403f906802fef019ea7f
出典データセット
uspto-grants-2014_04
特許番号
US08703700B2

反応ノート

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