Methoxyisopropylamine → HCID 86610350、化合物

HRID 1941755ノート

反応式

HRID 1941755 の反応式
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

参加物

7

反応物 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

生成物 1

HCID 86610350HCID 86610350、化合物

試薬・触媒・溶媒 2

HCID 9811564Bis(dibenzylideneacetone)palladium触媒HCID 1140Toluene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-02c8b15a9dad4a318dd81a2cb77af2ea
出典データセット
uspto-grants-2013_03
特許番号
US08389442B2

反応ノート

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