Acetic Acid → 4-{[(8-methoxy-4H-benzo[1,3]dioxin-6-yl)-(5-oxo-1-pyrimidin-2-yl-4,5-dihydro-1H-[1,2,4]triazol-3-yl)methyl]amino}benzamidine acetate

HRID 2079139

반응식

HRID 2079139 반응식
[CH3:1][O:2][C:3]1[C:12]2[O:11][CH2:10][O:9][CH2:8][C:7]=2[CH:6]=[C:5]([CH:13]([NH:26][C:27]2[CH:32]=[CH:31][C:30]([C:33]3[N:37]=C(C)O[N:34]=3)=[CH:29][CH:28]=2)[C:14]2[NH:15][C:16](=[O:25])[N:17]([C:19]3[N:24]=[CH:23][CH:22]=[CH:21][N:20]=3)[N:18]=2)[CH:4]=1.O.[C:40]([OH:43])(=[O:42])[CH3:41].FC(F)(F)C(O)=O.C(C1C=CC(NC(C2C=C(OC)C(OC)=CC=2F)C2NC(=O)N(C3C=CC=CC=3C(O)=O)N=2)=CC=1)(=N)N>CO.[Fe]>[C:40]([OH:43])(=[O:42])[CH3:41].[CH3:1][O:2][C:3]1[C:12]2[O:11][CH2:10][O:9][CH2:8][C:7]=2[CH:6]=[C:5]([CH:13]([NH:26][C:27]2[CH:32]=[CH:31][C:30]([C:33]([NH2:37])=[NH:34])=[CH:29][CH:28]=2)[C:14]2[NH:15][C:16](=[O:25])[N:17]([C:19]3[N:20]=[CH:21][CH:22]=[CH:23][N:24]=3)[N:18]=2)[CH:4]=1

참가 물질

7

반응물 4

HCID 176Acetic Acid2회HCID 962Water2회HCID 136173899HCID 136173899, 화합물HCID 1363370832-{3-[(4-carbamimidoylphenylamino)-(2-fluoro-4,5-dimethoxyphenyl)methyl]5-oxo-4,5-dihydro-[1,2,4]triazol-1-yl}benzoic Acid Trifluoroacetate

생성물 1

HCID 1356168544-{[(8-methoxy-4H-benzo[1,3]dioxin-6-yl)-(5-oxo-1-pyrimidin-2-yl-4,5-dihydro-1H-[1,2,4]triazol-3-yl)methyl]amino}benzamidine acetate

시약·촉매·용매 2

HCID 23925Iron촉매HCID 887Methanol용매2회

반응 조건

온도
60 °C

실험 절차

To a solution of 814 mg of 5-{(8-methoxy-4H-benzo[1,3]dioxin-6-yl)-[4-(5-methyl-[1,2,4]oxadiazol-3-yl)phenylamino]methyl}-2-pyrimidin-2-yl-2,4-dihydro-[1,2,4]triazol-3-one in 15 ml of a methanol:water:acetic acid=1:1:1 mixed solvent there was added 1g of iron powder, and the mixture was stirred overnight at 60° C. under a nitrogen atmosphere. After adding 7.5 ml of a methanol:water:acetic acid=1:1:1 mixed solvent to the reaction mixture, the mixture was further stirred at 60° C. for 5 hours. After filtering the reaction mixture, it was purified by reverse-phase high performance liquid chromatography (acetonitrile-water, 0.1% acetic acid) to give the title compound (476 mg).

후처리

  1. filtrationAfter filtering the reaction mixture, it
  2. customwas purified by reverse-phase high performance liquid chromatography (acetonitrile-water, 0.1% acetic acid)

출처 및 근거

ORD 기록
ord-af0c88505bd44b51852ebd22656c763c
출처 데이터셋
uspto-grants-2011_04
특허 번호
US07928228B2

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