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4-Isobutylbenzoic acid → Ethyl 5-[5-(4-isobutylphenyl)-1,2,4-oxadiazol-3-yl]pyrazine-2-carboxylate

HRID 2242224
ノート
印刷プレビュー

反応式

HRID 2242224 の反応式
[CH2:1]([C:5]1[CH:13]=[CH:12][C:8]([C:9]([OH:11])=O)=[CH:7][CH:6]=1)[CH:2]([CH3:4])[CH3:3].ON1C2C=CC=CC=2N=N1.F[B-](F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2C=CC=CC=2N=N1.C(N(C(C)C)CC)(C)C.[NH2:55][C:56](=[N:68]O)[C:57]1[N:58]=[CH:59][C:60]([C:63]([O:65][CH2:66][CH3:67])=[O:64])=[N:61][CH:62]=1>O1CCOCC1>[CH2:1]([C:5]1[CH:6]=[CH:7][C:8]([C:9]2[O:11][N:55]=[C:56]([C:57]3[N:58]=[CH:59][C:60]([C:63]([O:65][CH2:66][CH3:67])=[O:64])=[N:61][CH:62]=3)[N:68]=2)=[CH:12][CH:13]=1)[CH:2]([CH3:3])[CH3:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 381114-Isobutylbenzoic acidHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 136368376Ethyl 5-[amino(hydroxyimino)methyl]pyrazine-2-carboxylate

生成物 1

HCID 59204302
Ethyl 5-[5-(4-isobutylphenyl)-1,2,4-oxadiazol-3-yl]pyrazine-2-carboxylate
収率 27.1%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A mixture of 4-isobutylbenzoic acid (0.28 g, 1.59 mmol), 1-hydroxybenzotriazole (0.042 g, 0.31 mmol), N-[(1H-1,2,3-benzotriazol-1-yloxy)(dimethylamino)methylene]-N-methylmethanaminium tetrafluoroborate (0.51 g, 1.59 mmol), diisopropylethylamine (1.4 mL, 7.86 mmol) and dioxane (4 mL) was stirred at room temperature for 1 hour. Ethyl 5-[amino(hydroxyimino)methyl]pyrazine-2-carboxylate (0.33 g, 1.57 mmol) was added to the reaction mixture, stirred for 1.5 hours at room temperature and 6 hours at 100° C. The reaction mixture was cooled to room temperature, quenched with H2O (10 mL) and filtered. The precipitate was dissolved in EtOAc (10 mL), washed with 1N NaOH (3×10 mL) and brine (2×10 mL), dried (Na2SO4), filtered and concentrated in vacuo to yield the title compound (0.15 g, 27%) as a white solid.

後処理

  1. stirringstirred for 1.5 hours at room temperature and 6 hours at 100° C
  2. temperatureThe reaction mixture was cooled to room temperature
  3. customquenched with H2O (10 mL)
  4. filtrationfiltered
  5. dissolutionThe precipitate was dissolved in EtOAc (10 mL)
  6. washwashed with 1N NaOH (3×10 mL) and brine (2×10 mL)
  7. dry with materialdried (Na2SO4)
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-7ac23ec1106e409ca21bba6bb7fe27f3
出典データセット
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07671043B2

反応ノート

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