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Potassium Phosphate, Tribasic → HCID 118023460, 화합물

HRID 2171799
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HRID 2171799 반응식
Br[C:2]1[S:20][C:5]2[N:6]=[C:7]([CH3:19])[N:8]=[C:9]([CH2:10][N:11]3[CH2:16][CH2:15][S:14](=[O:18])(=[O:17])[CH2:13][CH2:12]3)[C:4]=2[CH:3]=1.CC1(C)C(C)(C)OB([C:29]2[CH2:36][CH2:35][C:32]3([CH2:34][CH2:33]3)[CH2:31][CH:30]=2)O1.C1(P(C2CCCCC2)C2C=CC=CC=2C2C(C(C)C)=CC(C(C)C)=CC=2C(C)C)CCCCC1.[O-]P([O-])([O-])=O.[K+].[K+].[K+]>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].O.O1CCOCC1>[O:17]=[S:14]1(=[O:18])[CH2:15][CH2:16][N:11]([CH2:10][C:9]2[C:4]3[CH:3]=[C:2]([C:29]4[CH2:36][CH2:35][C:32]5([CH2:34][CH2:33]5)[CH2:31][CH:30]=4)[S:20][C:5]=3[N:6]=[C:7]([CH3:19])[N:8]=2)[CH2:12][CH2:13]1
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참가 물질

8

반응물 4

HCID 62657Potassium Phosphate, TribasicHCID 111557942-Dicyclohexylphosphino-2',4',6'-triisoprophylbiphenylHCID 231425414,4,5,5-Tetramethyl-2-(spiro[2.5]oct-5-en-6-yl)-1,3,2-dioxaborolaneHCID 118023391HCID 118023391, 화합물

생성물 1

HCID 118023460HCID 118023460, 화합물수율 77.9%

시약·촉매·용매 3

HCID 9811564Bis(dibenzylideneacetone)palladium촉매
HCID 962Water용매2회
HCID 312751,4-Dioxane용매

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온도
100 °C

실험 절차

To a mixture of 6-bromo-4-[(1,1-dioxidothiomorpholin-4-yl)methyl]-2-methylthieno[2,3-d]pyrimidine (200 mg), 4,4,5,5-tetramethyl-2-(spiro[2.5]octa-5-en-6-yl)-1,3,2-dioxaborolane (185 mg), and dioxane (4 mL) were added Pd2dba3 (25 mg), dicyclohexyl (2′,4′,6′-triisopropylbiphenyl-2-yl)phosphine (50 mg), K3PO4 (340 mg), and water (200 μL), followed by heating and stirring at 100° C. overnight. The reaction mixture was cooled to room temperature, and water was added thereto, followed by extraction with EtOAc. The organic layer was dried over MgSO4, and then concentrated under reduced pressure. The residue was purified by a basic silica gel column (hexane/EtOAc) to obtain 4-[(1,1-dioxidothiomorpholin-4-yl)methyl]-2-methyl-6-(spiro[2.5]octa-5-en-6-yl)thieno[2,3-d]pyrimidine (167 mg).

후처리

  1. temperatureby heating
  2. temperatureThe reaction mixture was cooled to room temperature
  3. extractionfollowed by extraction with EtOAc
  4. dry with materialThe organic layer was dried over MgSO4
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by a basic silica gel column (hexane/EtOAc)

출처 및 근거

ORD 기록
ord-5e07215abbcc4d6bb45bd628622c9418
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09051339B2

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