反応式
[CH:1]1[CH:2]=[CH:3][C:4]2N(O)N=[N:7][C:5]=2C=1.CCN([CH:17]([CH3:19])C)C(C)C.CN([C:23]([O:27]N1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[Br:44]C1C(C(O)=O)=NC=CC=1.N1C=CN2CCNCC=12.[CH3:63][N:64]([CH:66]=[O:67])[CH3:65]>C(Cl)Cl>[Br:44][C:5]1[CH:4]=[CH:3][CH:2]=[C:1]([C:66]([N:64]2[CH2:65][CH2:19][C@@H:17]([O:27][CH3:23])[CH2:63]2)=[O:67])[N:7]=1参加物
8
反応物 6
HCID 6228Dimethylformamide
HCID 757711-Hydroxybenzotriazole
HCID 81531Diisopropylethylamine
HCID 20501293-Bromopyridine-2-carboxylic Acid
HCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)
HCID 132470465,6,7,8-Tetrahydroimidazo(1,2-a)pyrazine生成物 1
試薬・触媒・溶媒 1
実験手順
A solution of HOBt (148 mg, 0.97 mmol), DIEA (130 μL, 0.74 mmol), HATU (367 mg, 0.97 mmol), bromopyridine-2-carboxylic acid (150 mg, 0.74 mmol) and 5,6,7,8-tetrahydroimidazo[1,2-a]pyrazine (91 mg, 0.74 mmol) in DMF (2.5 mL) was stirred overnight at 65° C. Upon completion, Si-carbonate (2.8 g, 2.23 mmol) and DCM (3 mL) were added and the mixture was shaken overnight at room temperature. The resulting mixture was then filtered, washed with DCM, concentrated in vacuo and purified by reverse phase HPLC (acetonitrile/water+formic acid modifier) to afford the title compound.
後処理
- filtrationThe resulting mixture was then filtered
- washwashed with DCM
- concentrationconcentrated in vacuo
- custompurified by reverse phase HPLC (acetonitrile/water+formic acid modifier)
出典と根拠
- ORDレコード
- ord-ef6d136ec9034e4880c918885b1dd270
- 出典データセット
- uspto-grants-2013_02
- 特許番号
- US08367706B2
関連ノート
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