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Dichloromethane → HCID 86700204, 화합물

HRID 879397
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HRID 879397 반응식
Cl[C:2]1[CH:3]=[C:4]([C:8]2[CH:9]=[C:10]3[C:14](=[CH:15][CH:16]=2)[N:13]([CH3:17])[N:12]=[CH:11]3)[N:5]=[N:6][CH:7]=1.B1(B2OC(C)(C)C(C)(C)O2)OC(C)(C)C(C)(C)O1.ClCCl.C([O-])(=O)C.[K+].Br[C:45]1[S:46][C:47]2[C:53]([C:54]3[CH:59]=[CH:58][C:57]([Cl:60])=[CH:56][CH:55]=3)=[C:52]([C@H:61]([O:67][C:68]([CH3:71])([CH3:70])[CH3:69])[C:62]([O:64][CH2:65][CH3:66])=[O:63])[C:51]([CH3:72])=[CH:50][C:48]=2[N:49]=1.C([O-])([O-])=O.[K+].[K+]>C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[C:68]([O:67][C@@H:61]([C:52]1[C:51]([CH3:72])=[CH:50][C:48]2[N:49]=[C:45]([C:2]3[CH:3]=[C:4]([C:8]4[CH:9]=[C:10]5[C:14](=[CH:15][CH:16]=4)[N:13]([CH3:17])[N:12]=[CH:11]5)[N:5]=[N:6][CH:7]=3)[S:46][C:47]=2[C:53]=1[C:54]1[CH:55]=[CH:56][C:57]([Cl:60])=[CH:58][CH:59]=1)[C:62]([O:64][CH2:65][CH3:66])=[O:63])([CH3:69])([CH3:70])[CH3:71]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 6

HCID 6344DichloromethaneHCID 11430Potassium CarbonateHCID 517044Potassium AcetateHCID 2733548Bis(pinacolato)diboraneHCID 86700141(S)-ethyl 2-(2-bromo-7-(4-chlorophenyl)-5-methylbenzo[d]thiazol-6-yl)-2-tert-butoxyacetateHCID 867002035-(5-chloropyridazin-3-yl)-1-methyl-1H-indazole

생성물 1

HCID 86700204HCID 86700204, 화합물

시약·촉매·용매 1

HCID 178418397HCID 178418397, 화합물촉매

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온도
110 °C

실험 절차

5-(5-chloropyridazin-3-yl)-1-methyl-1H-indazole (75.0 mg, 0.307 mmol), bis(pinacolato)diboron (101.2 mg, 0.398 mmol), [1,1′Bis(diphenylphosphino)ferrocene]dichloropalladium(II) complex with dichloromethane (37.5 mg, 0.046 mmol), and potassium acetate (90.2 mg, 0.920 mmol) were taken in a microwave vial, and the vial was vacuum pumped and flushed with argon three times. To this mixture was added degassed DMF (3 mL). The reaction mixture was heated at 110° C. for 2 h then cooled. To the cooled reaction mixture was added (S)-ethyl 2-(2-bromo-7-(4-chlorophenyl)-5-methylbenzo[d]thiazol-6-yl)-2-tert-butoxyacetate (180.0 mg, 0.368 mmol), tetrakis(triphenylphosphine)palladium(0) (53.1 mg, 0.046 mmol), K2CO3 (127.1 mg, 0.920 mmol) and degassed water (0.5 mL). The reaction mixture was heated to 110° C. for 2 h, cooled, filtered through Celite (ethyl acetate eluent), and concentrated. Purification by flash column chromatography on silica gel (hexanes/ethyl acetate eluent) provided the product. LCMS-ESI+ calc'd for C34H33ClN5O3S (M+H+): 626.2; Found: 625.5 (M+H+).

후처리

  1. customflushed with argon three times
  2. additionTo this mixture was added
  3. customdegassed DMF (3 mL)
  4. temperaturethen cooled
  5. customTo the cooled reaction mixture
  6. customdegassed water (0.5 mL)
  7. temperatureThe reaction mixture was heated to 110° C. for 2 h
  8. temperaturecooled
  9. filtrationfiltered through Celite (ethyl acetate eluent)
  10. concentrationconcentrated
  11. customPurification by flash column chromatography on silica gel (hexanes/ethyl acetate eluent)
  12. customprovided the product

출처 및 근거

ORD 기록
ord-e9012eb478414b22ab142c8b44f47236
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08987250B2

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