Trifluoroacetic acid → HCID 131732882、化合物

HRID 578947

反応式

HRID 578947 の反応式
[CH2:1]([NH:8][C:9](=[O:18])[C:10]1[CH:15]=[CH:14][C:13]([NH:16][NH2:17])=N[CH:11]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CN(C)[CH:21]=[C:22]([C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][N:28]=1)[C:23]([O:25][CH3:26])=[O:24].[C:34](O)(C(F)(F)F)=O>C(O)C.CCOC(C)=O>[CH2:1]([NH:8][C:9]([C:10]1[CH:15]=[CH:14][C:13]([NH:16][NH:17][CH:21]=[C:22]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][N:28]=2)[C:23]([O:25][CH3:26])=[O:24])=[CH:34][CH:11]=1)=[O:18])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

6

反応物 3

HCID 6422Trifluoroacetic acidHCID 51370238N-benzyl-6-hydrazinylpyridine-3-carboxamideHCID 73047442Methyl 3-(dimethylamino)-2-(2-pyridinyl)-2-propenoate

生成物 1

HCID 131732882HCID 131732882、化合物収率 73.4%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Combined N-benzyl-6-hydrazinylnicotinamide (200 mg, 0.826 mmol), methyl 3-(dimethylamino)-2-(pyridin-2-yl)acrylate (170 mg, 0.826 mmol) and TFA (0.127 mL, 1.651 mmol) in ethanol (3 mL) and stirred overnight at room temperature. The reaction mixture was diluted in EtOAc (50 mL), washed with saturated aqueous sodium bicarbonate (20 ml), brine (20 ml), dried with Na2SO4 and concentrated to give the title compound (244 mg) as an orange solid, was used without further purification. MS m/z [M+H]+ 404.4.

後処理

  1. washwashed with saturated aqueous sodium bicarbonate (20 ml), brine (20 ml)
  2. dry with materialdried with Na2SO4
  3. concentrationconcentrated

出典と根拠

ORDレコード
ord-cbf05fdc8c4644d99ee17a5792b8df75
出典データセット
uspto-grants-2015_05
特許番号
US09040522B2

関連ノート

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