1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → 3-Amino-N-methylpyrazine-2-carboxamide

HRID 1887705ノート

反応式

HRID 1887705 の反応式
[NH2:1][C:2]1[C:3]([C:8]([OH:10])=O)=[N:4][CH:5]=[CH:6][N:7]=1.Cl.CN.C[CH2:15][N:16]=C=NCCCN(C)C.C1C=CC2N(O)N=NC=2C=1.CCN(C(C)C)C(C)C>CN(C=O)C.C(OCC)(=O)C>[NH2:1][C:2]1[C:3]([C:8]([NH:16][CH3:15])=[O:10])=[N:4][CH:5]=[CH:6][N:7]=1

参加物

8

反応物 5

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 726563-Amino-2-pyrazinecarboxylic acidHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 6364545Methylamine hydrochloride

生成物 1

HCID 108207483-Amino-N-methylpyrazine-2-carboxamide

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 3-aminopyrazine-2-carboxylic acid (965 mg, 6.94 mmol), methylamine hydrochloride (697 mg, 10.3 mmol), EDCI (1.61 g, 8.4 mmol), HOBt (1.136 g, 8.4 mmol) and DIEA (2.42 mL, 13.9 mmol) in DMF (24 mL) was stirred at room temperature for 48 h. It was diluted with ethyl acetate and washed with saturated sodium bicarbonate, brine and dried over magnesium sulfate. The solvent was removed and the residue was purified by silica gel chromatography (combiflash-companion; DCM/MeOH gradient) to give the title compound.

後処理

  1. washwashed with saturated sodium bicarbonate, brine
  2. dry with materialdried over magnesium sulfate
  3. customThe solvent was removed
  4. customthe residue was purified by silica gel chromatography (combiflash-companion; DCM/MeOH gradient)

出典と根拠

ORDレコード
ord-62bd56c7653e455a8870271bfe5ff7c9
出典データセット
uspto-grants-2013_08
特許番号
US08501763B2

反応ノート

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