1,2-Dichloroethane → HCID 178513834, 화합물

HRID 222005

반응식

HRID 222005 반응식
[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

참가 물질

8

반응물 5

HCID 111,2-DichloroethaneHCID 974Oxamic AcidHCID 6422Trifluoroacetic acidHCID 757711-HydroxybenzotriazoleHCID 178514300HCID 178514300, 화합물

생성물 1

HCID 178513834HCID 178513834, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 13387N-methyl-2-pyrrolidone용매

반응 조건

온도
150 °C

실험 절차

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.

후처리

  1. filtrationthe precipitate was collected by filtration

출처 및 근거

ORD 기록
ord-66a85126e86f4012a368f42eb2537669
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08207169B2

연결된 노트

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