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Potassium Carbonate → HCID 22938905、化合物

HRID 856623
ノート
印刷プレビュー

反応式

HRID 856623 の反応式
[SH:1][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][N:3]=1.Cl.Cl[CH2:13][C:14]1[N:18]([CH2:19][CH2:20][CH3:21])[CH:17]=[N:16][N:15]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[N+:8]([C:5]1[CH:6]=[CH:7][C:2]([S:1][CH2:13][C:14]2[N:18]([CH2:19][CH2:20][CH3:21])[CH:17]=[N:16][N:15]=2)=[N:3][CH:4]=1)([O-:10])=[O:9]
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 3

HCID 11430Potassium CarbonateHCID 229387553-chloromethyl-4-propyl-4H-1,2,4-triazole hydrochlorideHCID 178526723C5H4N2O2S

生成物 1

HCID 22938905HCID 22938905、化合物収率 89.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

2-mercapto-5-nitropyridine (5.0 g), 3-chloromethyl-4-propyl-4H-1,2,4-triazole hydrochloride (6.3 g) and potassium carbonate (11 g) was added to N,N-dimethylformamide (100 ml), and the mixture was stirred overnight at room temperature. The solvent was distilled off, and to the residue was added water, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was distilled off, to give 5-nitro-2-(4-propyl-4H-1,2,4-triazol-3-yl)methylthiopyridine (8.0 g) as brown crystals.

後処理

  1. distillationThe solvent was distilled off
  2. additionto the residue was added water
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with water and saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationThe solvent was distilled off

出典と根拠

ORDレコード
ord-80afcae74f2b4c1390683f6cd8ee6c51
出典データセット
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07262185B2

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