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Acetonitrile → HCID 178434074、化合物

HRID 659930
ノート
印刷プレビュー

反応式

HRID 659930 の反応式
[Cl:1][C:2]1[C:17]([O:18][CH2:19][CH2:20][N:21]2[CH:25]=[N:24][N:23]=[N:22]2)=[C:16]([Cl:26])[CH:15]=[CH:14][C:3]=1[C:4]([O:6]C1N(C)N=C(C)C=1)=O.C([N:29]([CH2:32][CH3:33])[CH2:30]C)C.CC(C)([OH:38])C#N.[C:40](#[N:42])[CH3:41]>>[Cl:1][C:2]1[C:17]([O:18][CH2:19][CH2:20][N:21]2[CH:25]=[N:24][N:23]=[N:22]2)=[C:16]([Cl:26])[CH:15]=[CH:14][C:3]=1[C:4]([C:33]1[C:40]([CH3:41])=[N:42][N:29]([CH3:30])[C:32]=1[OH:38])=[O:6]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 6342AcetonitrileHCID 6406Acetone CyanohydrinHCID 8471TriethylamineHCID 592816475-{2,4-Dichloro-3-[2-(1H-tetrazol-1-yl)ethyloxy]-benzoyloxy}-1,3-dimethylpyrazole

生成物 1

HCID 178434074HCID 178434074、化合物

実験手順

5-{2,4-Dichloro-3-[2-(1H-tetrazol-1-yl)ethyloxy]-benzoyloxy}-1,3-dimethylpyrazole (0.65 g) was dissolved in acetonitrile (10 ml), triethylamine (0.33 g) and acetone cyanohydrin (40 mg) were added thereto and the mixture was stirred at room temperature for 12 hours. The solvent was distilled off, acidified by the addition of diluted hydrochloric acid and extracted with ethyl acetate (150 ml). The organic layer was washed with saturated brine and dried with anhydrous magnesium sulfate. Ethyl acetate was distilled off to obtain objective 4-{2,4-dichloro-3-[2-(1H-tetrazol-1-yl)ethoxy]benzoyl}-1,3-dimethyl-5-hydroxy-pyrazole (0.59 g).

後処理

  1. distillationThe solvent was distilled off
  2. additionacidified by the addition of diluted hydrochloric acid
  3. extractionextracted with ethyl acetate (150 ml)
  4. washThe organic layer was washed with saturated brine
  5. dry with materialdried with anhydrous magnesium sulfate
  6. distillationEthyl acetate was distilled off

出典と根拠

ORDレコード
ord-4509f3115030417486da65d02160986c
出典データセット
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08084398B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート