Potassium Phosphate, Tribasic → HCID 70202778, 화합물

HRID 2367930노트

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HRID 2367930 반응식
[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

참가 물질

9

반응물 4

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

생성물 1

HCID 70202778HCID 70202778, 화합물

시약·촉매·용매 4

HCID 24290Palladium Chloride촉매HCID 962Water용매HCID 1140Toluene용매HCID 8857Ethyl Acetate용매

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온도
180 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-401dcfef1b1f403f906802fef019ea7f
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08703700B2

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