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Benzophenone imine → 6-Methoxy-5-(trifluoromethyl)pyridin-3-amine

HRID 1812395
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HRID 1812395 반응식
I[C:2]1[CH:3]=[C:4]([C:10]([F:13])([F:12])[F:11])[C:5]([O:8][CH3:9])=[N:6][CH:7]=1.CC1(C)C2C=CC=C(P(C3C=CC=CC=3)C3C=CC=CC=3)C=2OC2C1=CC=CC=2P(C1C=CC=CC=1)C1C=CC=CC=1.C1(C(C2C=CC=CC=2)=[NH:63])C=CC=CC=1.CC([O-])(C)C.[Na+]>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].CN(C=O)C>[CH3:9][O:8][C:5]1[N:6]=[CH:7][C:2]([NH2:63])=[CH:3][C:4]=1[C:10]([F:13])([F:12])[F:11]
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참가 물질

8

반응물 4

HCID 136809Benzophenone imineHCID 6360441,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)HCID 116880685-Iodo-2-methoxy-3-(trifluoromethyl)pyridineHCID 23676156Sodium t-butoxide

생성물 1

HCID 666004856-Methoxy-5-(trifluoromethyl)pyridin-3-amine수율 34%

시약·촉매·용매 3

HCID 9811564
Bis(dibenzylideneacetone)palladium
촉매
HCID 6228Dimethylformamide용매
HCID 8857Ethyl Acetate용매

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온도
120 °C

실험 절차

To 5-Iodo-2-methoxy-3-(trifluoromethyl)pyridine (0.97 g, 3.20 mmol) (ECA International Product List) was added DMF (8.0 mL), (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphine) (0.093 g, 0.160 mmol), Pd2(dba)3 (0.147 g, 0.160 mmol), diphenylmethanimine (0.806 mL, 4.80 mmol), and sodium 2-methylpropan-2-olate (1.231 g, 12.80 mmol), and the resulting mixture was heated at 120° C. for 30 min. The reaction mixture was then diluted with 100 mL of EtOAc, added to a separatory funnel, partitioned with 1 N HCl (aqueous), and washed 2 times with 50 mL of sodium bicarbonate (saturated, aqueous). The organic layer was separated, dried over sodium sulfate, and concentrated in vacuo. Chromatographic purification of the residue (silica gel, 0% to 5% (2 M ammonia in MeOH)/DCM) provided the title compound (34% yield). m/z (ESI, +ve ion) 193.2 (M+H)+.

후처리

  1. additionadded to a separatory funnel
  2. custompartitioned with 1 N HCl (aqueous)
  3. washwashed 2 times with 50 mL of sodium bicarbonate (saturated, aqueous)
  4. customThe organic layer was separated
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated in vacuo
  7. customChromatographic purification of the residue (silica gel, 0% to 5% (2 M ammonia in MeOH)/DCM)

출처 및 근거

ORD 기록
ord-2aa369e77bd54687a5db351182165e64
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08362241B2

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