Methoxyisopropylamine → HCID 86610350, 화합물

HRID 1941755노트

반응식

HRID 1941755 반응식
CC1(C)C2C(=C(P(C3C=CC=CC=3)C3C=CC=CC=3)C=CC=2)OC2C(P(C3C=CC=CC=3)C3C=CC=CC=3)=CC=CC1=2.Cl[C:44]1[CH:49]=[C:48]([C:50]2[CH:55]=[CH:54][N:53]=[C:52]([Cl:56])[CH:51]=2)[CH:47]=[CH:46][N:45]=1.[NH2:57][CH:58]([CH3:62])[CH2:59][O:60][CH3:61].CC(C)([O-])C.[Na+]>C1(C)C=CC=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.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[Cl:56][C:52]1[CH:51]=[C:50]([C:48]2[CH:47]=[CH:46][N:45]=[C:44]([NH:57][CH:58]([CH3:62])[CH2:59][O:60][CH3:61])[CH:49]=2)[CH:55]=[CH:54][N:53]=1

참가 물질

7

반응물 4

HCID 123458MethoxyisopropylamineHCID 6360441,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)HCID 51720972,2'-dichloro-4,4'-bipyridineHCID 23676156Sodium t-butoxide

생성물 1

HCID 86610350HCID 86610350, 화합물

시약·촉매·용매 2

HCID 9811564Bis(dibenzylideneacetone)palladium촉매HCID 1140Toluene용매

실험 절차

Xantphos (32 mg), and Pd2(dba)3 (25 mg) were suspended in toluene (8 ml) and stirred under argon for 10 mins, then 2,2′-dichloro-[4,4′]-bipyridinyl (250 mg), 2-amino-1-methoxypropane (0.117 ml) and sodium tert-butoxide (150 mg) were added. The mixture stirred at 60° C. for 6 hours then cooled to room temp, poured onto water and extracted with ethyl acetate, dried over Na2SO4 and concentrated under reduced pressure. The residue was purified by passing the crude mixture down Kieselgel using a gradient of hexane and ethyl acetate as the eluent.

후처리

  1. stirringThe mixture stirred at 60° C. for 6 hours
  2. additionpoured onto water
  3. extractionextracted with ethyl acetate
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified

출처 및 근거

ORD 기록
ord-02c8b15a9dad4a318dd81a2cb77af2ea
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08389442B2

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