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Potassium Phosphate, Tribasic → 4-cyclopropyl-N-(3-(dimethylamino)propyl)-N-methyl-2-nitrobenzenamine

HRID 502740
ノート
印刷プレビュー

反応式

HRID 502740 の反応式
C1(B2O[C:7]([CH3:10])([CH3:9])[C:6]([CH3:12])([CH3:11])O2)CC1.P([O-])([O-])([O-])=O.[K+].[K+].[K+].BrC1C=[CH:26][C:25]([N:28]([CH3:35])[CH2:29][CH2:30][CH2:31][N:32]([CH3:34])[CH3:33])=[C:24]([N+:36]([O-:38])=[O:37])C=1.C1(P(C2CCCCC2)C2CCCCC2)CCCCC1>C([O-])(=O)C.[Pd+2].C([O-])(=O)C.C1(C)C=CC=CC=1.O>[CH:6]1([C:7]2[CH:9]=[CH:26][C:25]([N:28]([CH2:29][CH2:30][CH2:31][N:32]([CH3:34])[CH3:33])[CH3:35])=[C:24]([N+:36]([O-:38])=[O:37])[CH:10]=2)[CH2:11][CH2:12]1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 62657Potassium Phosphate, TribasicHCID 75806TricyclohexylphosphineHCID 27580152-Cyclopropyl-4,4,5,5-tetramethyl-1,3,2-dioxaborolaneHCID 16109013HCID 16109013、化合物

生成物 1

HCID 161090144-cyclopropyl-N-(3-(dimethylamino)propyl)-N-methyl-2-nitrobenzenamine

試薬・触媒・溶媒 3

HCID 167845
palladium(II) acetate
触媒
HCID 962Water溶媒
HCID 1140Toluene溶媒

実験手順

To a pressure vessel was added 2-cyclopropyl-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (900 mg, 5.36 mmol), potassium phosphate (3.0 g, 14.42 mmol), and 0.82 mL water. After stirring at RT for 15 minutes, N-(4-Bromo-2-nitro-phenyl)-N,N′,N′-trimethyl-propane-1,3-diamine (Step 1, 1.30 g, 4.12 mmol), palladium acetate (92 mg, 0.412 mmol), tricyclohexylphosphine (231 mg 0.824 mmol), and 21 ml toluene were added. The reaction was sealed and stirred at 80° C. for 19 h. The reaction was then cooled to RT, quenched with EtOAc and extracted into water, washed once with brine, and then dried over Mg2SO4. The crude mixture was then purified by reverse phase chromatography to yield the title compound as a dark red-brown oil. MS (M+H+)=278; Calc'd for C15H23N3O2=277.36.

後処理

  1. customThe reaction was sealed
  2. stirringstirred at 80° C. for 19 h
  3. temperatureThe reaction was then cooled to RT
  4. customquenched with EtOAc
  5. extractionextracted into water
  6. washwashed once with brine
  7. dry with materialdried over Mg2SO4
  8. customThe crude mixture was then purified by reverse phase chromatography

出典と根拠

ORDレコード
ord-d37d050ab4b8446cb68e41ee0dd0977e
出典データセット
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07776869B2

反応ノート

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