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tert-Butyl carbamate → tert-butyl 6-(5-methoxy-1-methyl-1H-indol-3-yl)-5-((2-(trimethylsilyl)ethoxy)methyl)-5H-pyrrolo[2,3-b]pyrazin-2-ylcarbamate

HRID 1628038
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HRID 1628038 반응식
C(P(C(C)(C)C)C1C=CC=CC=1C1C(C(C)C)=CC(C(C)C)=CC=1C(C)C)(C)(C)C.Br[C:32]1[N:33]=[C:34]2[CH:40]=[C:39]([C:41]3[C:49]4[C:44](=[CH:45][CH:46]=[C:47]([O:50][CH3:51])[CH:48]=4)[N:43]([CH3:52])[CH:42]=3)[N:38]([CH2:53][O:54][CH2:55][CH2:56][Si:57]([CH3:60])([CH3:59])[CH3:58])[C:35]2=[N:36][CH:37]=1.[C:61](=[O:68])([O:63][C:64]([CH3:67])([CH3:66])[CH3:65])[NH2:62].CC([O-])(C)C.[Na+]>O1CCOCC1.CCOC(C)=O.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]>[CH3:51][O:50][C:47]1[CH:48]=[C:49]2[C:44](=[CH:45][CH:46]=1)[N:43]([CH3:52])[CH:42]=[C:41]2[C:39]1[N:38]([CH2:53][O:54][CH2:55][CH2:56][Si:57]([CH3:60])([CH3:59])[CH3:58])[C:35]2=[N:36][CH:37]=[C:32]([NH:62][C:61](=[O:68])[O:63][C:64]([CH3:67])([CH3:66])[CH3:65])[N:33]=[C:34]2[CH:40]=1
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8

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HCID 77922tert-Butyl carbamateHCID 11618717Di-tert-butyl(2',4',6'-tris(propan-2-yl)-(1,1'-biphenyl)-2-yl)phosphaneHCID 23676156Sodium t-butoxideHCID 580101552-bromo-6-(5-methoxy-1-methyl-1H-indol-3-yl)-5-((2-(trimethylsilyl)ethoxy)methyl)-5H-pyrrolo[2,3-b]pyrazine

생성물 1

HCID 67216771
tert-butyl 6-(5-methoxy-1-methyl-1H-indol-3-yl)-5-((2-(trimethylsilyl)ethoxy)methyl)-5H-pyrrolo[2,3-b]pyrazin-2-ylcarbamate
수율 42%

시약·촉매·용매 3

HCID 9811564Bis(dibenzylideneacetone)palladium촉매HCID 8857Ethyl Acetate용매HCID 312751,4-Dioxane용매

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온도
80 °C

실험 절차

In a flask was added Pd2(dba)3 (0.094 g, 0.10 mmol) and di-tert-butyl(2′,4′,6′-triisopropylbiphenyl-2-yl)phosphine (0.087 g, 0.21 mmol) in 1,4-dioxane (10 mL). The mixture was heated to about 80° C. for about 10 min. 2-Bromo-6-(5-methoxy-1-methyl-1H-indol-3-yl)-5-((2-(trimethylsilyl)ethoxy)methyl)-5H-pyrrolo[2,3-b]pyrazine (0.500 g, 1.03 mmol, Preparation #C.1), tert-butyl carbamate (0.180 g, 1.54 mmol) and NaOt-Bu (0.148 g, 1.54 mmol) were then added and heating was continued for about 45 min. The mixture was cooled to rt and diluted with EtOAc (20 mL), washed with water (15 mL) and dried over MgSO4. The mixture was filtered and concentrated in vacuo and purified by a 12 g silica column eluting with 0 to 30% EtOAc/DCM to provide tert-butyl 6-(5-methoxy-1-methyl-1H-indol-3-yl)-5-((2-(trimethylsilyl)ethoxy)methyl)-5H-pyrrolo[2,3-b]pyrazin-2-ylcarbamate (0.224 g, 42%): LC/MS (Table 2, Method g) Rt=1.99 min; MS m/z 524 (M+H)+.

후처리

  1. temperatureheating
  2. temperatureThe mixture was cooled to rt
  3. washwashed with water (15 mL)
  4. dry with materialdried over MgSO4
  5. filtrationThe mixture was filtered
  6. concentrationconcentrated in vacuo
  7. custompurified by a 12 g silica column
  8. washeluting with 0 to 30% EtOAc/DCM

출처 및 근거

ORD 기록
ord-6c473d0737744f40bcb1c4220d5103df
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08785639B2

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