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Potassium Phosphate, Tribasic → HCID 86708290, 화합물

HRID 538892
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HRID 538892 반응식
Br[C:2]1[S:3][C:4]2[CH:10]=[C:9]([CH2:11][CH2:12][CH2:13][CH3:14])[CH:8]=[CH:7][C:5]=2[N:6]=1.[CH3:15][O:16][C:17]([C:19]1[CH:24]=[CH:23][C:22](B(O)O)=[CH:21][CH:20]=1)=[O:18].CC(C1C=C(C(C)C)C(C2C=CC=CC=2P(C2CCCCC2)C2CCCCC2)=C(C(C)C)C=1)C.P([O-])([O-])([O-])=[O:63].[K+].[K+].[K+]>O1CCOCC1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[C:11]([C:9]1[CH:8]=[CH:7][C:5]2[N:6]=[C:2]([C:22]3[CH:23]=[CH:24][C:19]([C:17]([O:16][CH3:15])=[O:18])=[CH:20][CH:21]=3)[S:3][C:4]=2[CH:10]=1)(=[O:63])[CH2:12][CH2:13][CH3:14]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 62657Potassium Phosphate, TribasicHCID 27343694-Methoxycarbonylphenylboronic acidHCID 111557942-Dicyclohexylphosphino-2',4',6'-triisoprophylbiphenylHCID 866818992-Bromo-6-butylbenzo[d]thiazole

생성물 1

HCID 86708290HCID 86708290, 화합물

시약·촉매·용매 2

HCID 9811564
Bis(dibenzylideneacetone)palladium
촉매
HCID 312751,4-Dioxane용매

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온도
100 °C

실험 절차

Step-4: A degassed mixture of 2-bromo-6-butylbenzo[d]thiazole (142 mg, 0.5 mmol), (4-(methoxycarbonyl)phenyl)boronic acid (135 mg, 0.75 mmol), Pd2(dba)3 (9 mg, 0.01 mmol), Xphos (9.5 mg, 0.02 mmol), potassium phosphate (207 mg, 1.5 mmol) in dioxane (2 mL) under nitrogen atmosphere was stirred at 100° C. for 6 h. The reaction mixture was cooled to RT, evaporated and extracted with dichloromethane, washed with brine, dried over anhydrous sodium sulfate and evaporated. The crude product was purified by preparative TLC to afford methyl 4-(6-butyrylbenzo[d]thiazol-2-yl)benzoate, MS (ESI+) m/z 340.2 [M+1]+

후처리

  1. temperatureThe reaction mixture was cooled to RT
  2. customevaporated
  3. extractionextracted with dichloromethane
  4. washwashed with brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. customevaporated
  7. customThe crude product was purified by preparative TLC

출처 및 근거

ORD 기록
ord-ee5a7f86321b4f1199f62195355acbca
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08865752B2

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