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Cesium carbonate → Darigabat

HRID 1845984
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HRID 1845984 반응식
[CH2:1]([N:3]1[C:7]2[N:8]=[N:9][CH:10]=[C:11]([C:12]3[CH:17]=[CH:16][C:15]([F:18])=[C:14](I)[CH:13]=3)[C:6]=2[N:5]=[CH:4]1)[CH3:2].[CH2:20]([S:22]([C:25]1[CH:30]=[CH:29][C:28](B2OC(C)(C)C(C)(C)O2)=[C:27]([O:40][CH3:41])[CH:26]=1)(=[O:24])=[O:23])[CH3:21].C(=O)([O-])[O-].[Cs+].[Cs+]>O1CCOCC1.O.CCOC(C)=O.[Pd](Cl)Cl.C(P(C(C)(C)C)[C-]1C=CC=C1)(C)(C)C.[C-]1(P(C(C)(C)C)C(C)(C)C)C=CC=C1.[Fe+2]>[CH2:1]([N:3]1[C:7]2[N:8]=[N:9][CH:10]=[C:11]([C:12]3[CH:13]=[C:14]([C:28]4[CH:29]=[CH:30][C:25]([S:22]([CH2:20][CH3:21])(=[O:24])=[O:23])=[CH:26][C:27]=4[O:40][CH3:41])[C:15]([F:18])=[CH:16][CH:17]=3)[C:6]=2[N:5]=[CH:4]1)[CH3:2]
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참가 물질

8

반응물 3

HCID 10796Cesium carbonateHCID 867232067-ethyl-4-(4-fluoro-3-iodophenyl)-7H-imidazo[4,5-c]pyridazineHCID 867232082-(4-(Ethylsulfonyl)-2-methoxyphenyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane

생성물 1

HCID 76287260Darigabat수율 13%

시약·촉매·용매 4

HCID 178454861HCID 178454861, 화합물
촉매
HCID 962Water용매
HCID 8857Ethyl Acetate용매
HCID 312751,4-Dioxane용매

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온도
100 °C

실험 절차

A stirred solution of 7-ethyl-4-(4-fluoro-3-iodophenyl)-7H-imidazo[4,5-c]pyridazine (Preparation 10, 100 mg, 0.27 mmol), 2-(4-ethylsulfonyl-2-methoxyphenyl)-4,4,5,5-tetramethyl-[1,3,2]dioxaborolane (Preparation 21, 88 mg, 0.27 mmol) and cesium carbonate (177 mg, 0.54 mmol) in dioxane (5 mL) and water (1 mL) was degassed with argon for 10 minutes followed by the addition of 1,1′-bis(di-tert-butylphosphino) ferrocene palladium dichloride (4.4 mg, 0.005 mmol). The resulting mixture was heated at 100° C. for 16 hours, cooled to room temperature and diluted with EtOAc (15 mL). The organic layer was washed with water (10 mL) and saturated brine solution (10 mL) then dried over Na2SO4, filtered and concentrated in vacuo. Purification by silica gel column chromatography eluting with CH2Cl2:MeOH 98:2 afforded the title compound as off white solid in 13% yield, 15 mg.

후처리

  1. temperaturecooled to room temperature
  2. washThe organic layer was washed with water (10 mL) and saturated brine solution (10 mL)
  3. dry with materialthen dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customPurification by silica gel column chromatography
  7. washeluting with CH2Cl2:MeOH 98:2

출처 및 근거

ORD 기록
ord-20ef1c37707545e0a1eeb22faa8d4006
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08952008B2

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