Diisopropylethylamine → HCID 71117227、化合物

HRID 629887

反応式

HRID 629887 の反応式
[NH2:1][CH:2]1[CH2:7][CH2:6][C:5]([C:8]2[N:13]=[C:12]3[N:14]([CH3:23])[C:15](=[O:22])[N:16]([CH2:17][C:18]([CH3:21])([CH3:20])[CH3:19])[C:11]3=[CH:10][CH:9]=2)=[CH:4][CH2:3]1.CCN(C(C)C)C(C)C.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[CH3:57][N:58]1[CH:62]=[CH:61][N:60]=[C:59]1[C:63](O)=[O:64]>CN1C(=O)CCC1>[CH3:21][C:18]([CH3:20])([CH3:19])[CH2:17][N:16]1[C:11]2[C:12](=[N:13][C:8]([C:5]3[CH2:6][CH2:7][CH:2]([NH:1][C:63]([C:59]4[N:58]([CH3:57])[CH:62]=[CH:61][N:60]=4)=[O:64])[CH2:3][CH:4]=3)=[CH:9][CH:10]=2)[N:14]([CH3:23])[C:15]1=[O:22]

参加物

6

反応物 4

HCID 81531DiisopropylethylamineHCID 5576781-methyl-1H-imidazole-2-carboxylic acidHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 71117107HCID 71117107、化合物

生成物 1

HCID 71117227HCID 71117227、化合物

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

To a round bottom flask were added 5-(4-Aminocyclohex-1-en-1-yl)-1-(2,2-dimethylpropyl)-3-methyl-1,3-dihydro-2H-imidazo[4,5-b]pyridin-2-one (17-2) (0.0010 g, 0.028 mmol), DIPEA (0.050 mL, 0.286 mmol), HATU (0.0013 g, 0.034 mmol), 1-methyl-1H-imidazole-2-carboxylic acid (0.00467 g, 0.037 mmol), and NMP (1 mL). The reaction was stirred at room temperature overnight (˜14 hours), the reaction mixtures were then filtered & purified by reverse-phase chromatography (5-95% 0.1% TFA in H2O:acetonitrile) to give N-{4-[1-(2,2-Dimethylpropyl)-3-methyl-2-oxo-2,3-dihydro-1H-imidazo[4,5-b]pyridin-5-yl]cyclohex-3-en-1-yl}-1-methyl-1H-imidazole-2-carboxamide (17-3). HRMS m/z (M+H): calculated=423.2503; observed=423.2507.

後処理

  1. customthe reaction mixtures
  2. filtrationwere then filtered
  3. custompurified by reverse-phase chromatography (5-95% 0.1% TFA in H2O:acetonitrile)

出典と根拠

ORDレコード
ord-8e10d4badbc643879d71b710f9e661e0
出典データセット
uspto-grants-2016_04
特許番号
US09315518B2

関連ノート

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