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Sodium Acetate → HCID 10117620、化合物

HRID 1791123
ノート
印刷プレビュー

反応式

HRID 1791123 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[CH:9]=[C:10]([C:15](=O)[CH2:16][CH2:17][N:18]1[CH2:22][CH2:21][S:20][CH2:19]1)[C:11]([O:13][CH3:14])=[O:12].Cl.[F:25][C:26]1[C:27]([C:33](=[NH:35])[NH2:34])=[N:28][CH:29]=[C:30]([F:32])[CH:31]=1.C([O-])(=O)C.[Na+]>C(O)(C)C>[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[CH:9]1[C:10]([C:11]([O:13][CH3:14])=[O:12])=[C:15]([CH2:16][CH2:17][N:18]2[CH2:22][CH2:21][S:20][CH2:19]2)[NH:35][C:33]([C:27]2[C:26]([F:25])=[CH:31][C:30]([F:32])=[CH:29][N:28]=2)=[N:34]1
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 517045Sodium AcetateHCID 220278403,5-Difluoropyridine-2-carboximidamide--hydrogen chloride (1/1)HCID 69588140HCID 69588140、化合物

生成物 1

HCID 10117620HCID 10117620、化合物

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

A solution of 0.20 g (0.56 mmol) of the compound from Example IX in 5 ml of isopropanol is heated together with 0.11 g (0.56 mmol) of the compound from Example VI and 0.06 g (0.67 mmol) of sodium acetate under reflux for 2 hours. The reaction mixture is concentrated, and the residue is taken up in ethyl acetate and extracted with dilute hydrochloric acid. The aqueous phase is made alkaline with dilute sodium hydroxide solution and extracted with ethyl acetate. The organic phase is dried over sodium sulfate and concentrated. The residue is chromatographed on silica gel with cyclohexane/ethyl acetate (5:1→3:1) as mobile phase.

後処理

  1. temperatureunder reflux for 2 hours
  2. concentrationThe reaction mixture is concentrated
  3. extractionextracted with dilute hydrochloric acid
  4. extractionextracted with ethyl acetate
  5. dry with materialThe organic phase is dried over sodium sulfate
  6. concentrationconcentrated
  7. customThe residue is chromatographed on silica gel with cyclohexane/ethyl acetate (5:1→3:1) as mobile phase

出典と根拠

ORDレコード
ord-2fba051fc5664ebf804df2ddb251efca
出典データセット
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07074784B2

反応ノート

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