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Potassium Phosphate, Tribasic → HCID 68328656, 화합물

HRID 634233
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HRID 634233 반응식
[C:1]([NH:5][C:6]1[O:7][C:8]([C:11]2[CH:12]=[C:13]3[C:17](=[CH:18][CH:19]=2)[N:16]([S:20]([C:23]2[CH:29]=[CH:28][C:26]([CH3:27])=[CH:25][CH:24]=2)(=[O:22])=[O:21])[CH:15]=[C:14]3B2OC(C)(C)C(C)(C)O2)=[N:9][N:10]=1)([CH3:4])([CH3:3])[CH3:2].Cl[C:40]1[N:45]=[C:44]([CH:46]2[CH2:48][CH2:47]2)[C:43]([F:49])=[CH:42][N:41]=1.P([O-])([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].C1(P(C2CCCCC2)C2C=CC=CC=2C2C(C(C)C)=CC(C(C)C)=CC=2C(C)C)CCCCC1>[C:1]([NH:5][C:6]1[O:7][C:8]([C:11]2[CH:12]=[C:13]3[C:17](=[CH:18][CH:19]=2)[N:16]([S:20]([C:23]2[CH:29]=[CH:28][C:26]([CH3:27])=[CH:25][CH:24]=2)(=[O:22])=[O:21])[CH:15]=[C:14]3[C:40]2[N:45]=[C:44]([CH:46]3[CH2:48][CH2:47]3)[C:43]([F:49])=[CH:42][N:41]=2)=[N:9][N:10]=1)([CH3:4])([CH3:2])[CH3:3]
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참가 물질

6

반응물 3

HCID 62657Potassium Phosphate, TribasicHCID 68328226HCID 68328226, 화합물HCID 772310692-chloro-4-cyclopropyl-5-fluoroPyrimidine

생성물 1

HCID 68328656HCID 68328656, 화합물수율 76.4%

시약·촉매·용매 2

HCID 9811564Bis(dibenzylideneacetone)palladium촉매
HCID 11155794
2-Dicyclohexylphosphino-2',4',6'-triisoprophylbiphenyl
촉매

반응 조건

온도
130 °C

실험 절차

To a 5 mL glass microwave tube containing N-tert-butyl-5-(3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1-tosyl-1H-indol-5-yl)-1,3,4-oxadiazol-2-amine (166 mg, 0.309 mmol) was added 2-chloro-4-cyclopropyl-5-fluoropyrimidine (69.4 mg, 0.402 mmol), potassium phosphate (197 mg, 0.928 mmol), dicyclohexyl(2′,4′,6′-triisopropylbiphenyl-2-yl)phosphine (8.9 mg, 0.019 mmol), and Pd2(dba)3 (8.5 mg, 9.28 μmol). The tube was purged with argon, the solids were treated with dioxane (3 mL) and Water (0.3 mL), the tube was sealed, and the contents were heated in an Initiator microwave reactor (Personal Chemistry, Biotage AB, Inc., Upssala, Sweden) at 130° C. for 30 min. The mixture was treated with H2O and extracted with EtOAc. The organic layer was washed with brine, dried over MgSO4, filtered and concentrated. The crude material was purified by flash chromatography (eluting with 5-60% EtOAc in Hex) affording N-tert-butyl-5-(3-(4-cyclopropyl-5-fluoropyrimidin-2-yl)-1-tosyl-1H-indol-5-yl)-1,3,4-oxadiazol-2-amine (129 mg, 76%) as a light yellow viscous oil. MS (ESI, pos. ion) m/z: 547.1 (M+1).

후처리

  1. customThe tube was purged with argon
  2. additionthe solids were treated with dioxane (3 mL) and Water (0.3 mL)
  3. customthe tube was sealed
  4. additionThe mixture was treated with H2O
  5. extractionextracted with EtOAc
  6. washThe organic layer was washed with brine
  7. dry with materialdried over MgSO4
  8. filtrationfiltered
  9. concentrationconcentrated
  10. customThe crude material was purified by flash chromatography (eluting with 5-60% EtOAc in Hex)

출처 및 근거

ORD 기록
ord-223bb0c07b54402da046e3e6967b2c81
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09321756B2

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