1,2-Dichloroethane → HCID 178513834、化合物

HRID 222005

反応式

HRID 222005 の反応式
[NH:1]([C:3]1[CH:4]=[CH:5][C:6]2[C:7]([N:19]=1)=[N:8][C:9]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)=[C:10]([OH:12])[N:11]=2)[NH2:2].C1C=CC2N(O)N=NC=2C=1.[C:30](O)(=O)[C:31]([NH2:33])=[O:32].C(Cl)CCl.C(O)(C(F)(F)F)=O>CN1C(=O)CCC1.O>[OH:12][C:10]1[N:11]=[C:6]2[CH:5]=[CH:4][C:3]3=[N:1][N:2]=[C:30]([C:31]([NH2:33])=[O:32])[N:19]3[C:7]2=[N:8][C:9]=1[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

参加物

8

反応物 5

HCID 111,2-DichloroethaneHCID 974Oxamic AcidHCID 6422Trifluoroacetic acidHCID 757711-HydroxybenzotriazoleHCID 178514300HCID 178514300、化合物

生成物 1

HCID 178513834HCID 178513834、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
150 °C

実験手順

To a mixture of 6-hydrazinyl-3-phenylpyrido[2,3-b]pyrazin-2(1H)-one (3-3) (300 mg, 1.19 mmol), HOBt (218 mg, 1.42 mmol) and oxamic acid (130 mg, 1.42 mmol) in NMP (12 mL) was added EDC (272 mg, 1.42 mmol) at room temperature and the mixture was stirred for 30 min. After addition of TFA (0.091 mL, 1.19 mmol), the mixture was heated under microwave irradiation at 150° C. for 30 minutes. To a mixture was added water (60 mL) and the precipitate was collected by filtration to give 3-hydroxy-2-phenyl[1,2,4]triazolo[4′,3′:1,6]pyrido[2,3-b]pyrazin-9-carboxamide (9-1) as a yellow powder.

後処理

  1. filtrationthe precipitate was collected by filtration

出典と根拠

ORDレコード
ord-66a85126e86f4012a368f42eb2537669
出典データセット
uspto-grants-2012_06
特許番号
US08207169B2

関連ノート

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