Sodium Chloride → HCID 47298773、化合物

HRID 241284

反応式

HRID 241284 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([S:8](Cl)(=[O:10])=[O:9])=[CH:4][CH:3]=1.Cl.[C:13]([C:15]1[CH:22]=[CH:21][C:18]([CH2:19][NH2:20])=[CH:17][CH:16]=1)#[N:14].[Cl-].[Na+]>>[C:13]([C:15]1[CH:22]=[CH:21][C:18]([CH2:19][NH:20][S:8]([C:5]2[CH:6]=[CH:7][C:2]([F:1])=[CH:3][CH:4]=2)(=[O:10])=[O:9])=[CH:17][CH:16]=1)#[N:14]

参加物

4

反応物 3

HCID 5234Sodium ChlorideHCID 95884-Fluorobenzenesulfonyl chlorideHCID 99422504-(Aminomethyl)benzonitrile hydrochloride

生成物 1

HCID 47298773HCID 47298773、化合物収率 89.5%

実験手順

Reaction was carried out in the same manner as in a Reference Example 2-(d) except for using 4-fluorobenzenesulfonyl chloride (1.18 g, 6.06 mmol) in place of 3-pyridylsulfonyl chloride, and using 4-cyanobenzylamine hydrochloride (1.00 g, 5.93 mmol) in place of (6-phenylpyridazin-3-ylmethyl)amine hydrochloride. After completion of the reaction, a saturated aqueous sodium chloride solution was added to the reaction solution, followed by extraction with ethyl acetate. The separated organic layer was dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. To the resulting residue dissolved in a small amount of methylene chloride was added hexane, and a precipitated solid was collected by filtration. The resulting solid was dried under reduced pressure at 60° C. to afford the title compound (1.54 g) as a slightly brown solid. (Yield: 89%)

後処理

  1. customReaction
  2. customAfter completion of the reaction
  3. extractionfollowed by extraction with ethyl acetate
  4. dry with materialThe separated organic layer was dried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. dissolutionTo the resulting residue dissolved in a small amount of methylene chloride
  7. additionwas added hexane
  8. filtrationa precipitated solid was collected by filtration
  9. customThe resulting solid was dried under reduced pressure at 60° C.

出典と根拠

ORDレコード
ord-4f48ed52527942d3a31f8956d81718e2
出典データセット
uspto-grants-2014_02
特許番号
US08648097B2

関連ノート

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