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2-Aminopyridine-4-carbohydrazide → (3-{5-amino-6-[3-(2-aminopyridin-4-yl)-1H-1,2,4-triazol-5-yl]pyrazin-2-yl}phenyl)methanol

HRID 646759
ノート
印刷プレビュー

反応式

HRID 646759 の反応式
[NH2:1][C:2]1[C:3]([C:16]#[N:17])=[N:4][C:5]([C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([CH2:14][OH:15])[CH:9]=2)=[CH:6][N:7]=1.[NH2:18][C:19]1[CH:20]=[C:21]([CH:26]=[CH:27][N:28]=1)[C:22]([NH:24][NH2:25])=O>CN(C=O)C>[NH2:1][C:2]1[N:7]=[CH:6][C:5]([C:8]2[CH:9]=[C:10]([CH2:14][OH:15])[CH:11]=[CH:12][CH:13]=2)=[N:4][C:3]=1[C:16]1[NH:25][N:24]=[C:22]([C:21]2[CH:26]=[CH:27][N:28]=[C:19]([NH2:18])[CH:20]=2)[N:17]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 3225522-Aminopyridine-4-carbohydrazideHCID 587105723-Amino-6-[3-(hydroxymethyl)phenyl]pyrazine-2-carbonitrile

生成物 1

HCID 68650742(3-{5-amino-6-[3-(2-aminopyridin-4-yl)-1H-1,2,4-triazol-5-yl]pyrazin-2-yl}phenyl)methanol収率 5.8%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
180 °C

実験手順

To a solution of of 3-amino-6-[3-(hydroxymethyl)phenyl]pyrazine-2-carbonitrile (250 mg, 1.11 mmol) was added 2-aminoisonicotinic acid hydrazide (311 mg, 2.04 mmol). After being heated at 180° C. for 90 min, the reaction mixture was dissolved in DMF and washed with water, ethyl acetate (10 mL×3). The aqueous phase was extracted once with additional ethyl acetate. The combined organic layers were washed with saturated aqueous sodium chloride then dried over anhydrous magnesium sulfate. Filtration and concentration in vacuo gave a crude oil, which was purified by preparative HPLC to yield (3-{5-amino-6-[3-(2-aminopyridin-4-yl)-1H-1,2,4-triazol-5-yl]pyrazin-2-yl}phenyl)methanol (23.2 mg, 5.7% yield): 1H NMR (400 MHz, DMSO-d6): δ 8.80 (s, 1H), 8.15 (s, 1H), 8.10 (m, 1H), 7.70 (m, 2H), 7.43 (m, 2H), 7.20 (m, 1H), 6.10 (s, 2H), 5.25 (m, 1H) 4.60 (m, 1H); MS (EI) for C18H16N8O: 361.11 (MH+).

後処理

  1. washwashed with water, ethyl acetate (10 mL×3)
  2. extractionThe aqueous phase was extracted once with additional ethyl acetate
  3. washThe combined organic layers were washed with saturated aqueous sodium chloride
  4. dry with materialthen dried over anhydrous magnesium sulfate
  5. filtrationFiltration and concentration in vacuo
  6. customgave a crude oil, which
  7. customwas purified by preparative HPLC

出典と根拠

ORDレコード
ord-0c65b7c9be9b476cabcae692e896ca8c
出典データセット
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07704995B2

反応ノート

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