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Sodium Carbonate → Methyl 2-chloro-3-hydroxyiminomethyl-4-methylsulfonylbenzoate

HRID 322055
ノート
印刷プレビュー

反応式

HRID 322055 の反応式
[Cl:1][C:2]1[C:11]([CH:12]=O)=[C:10]([S:14]([CH3:17])(=[O:16])=[O:15])[CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5].[Cl-].[OH:19][NH3+:20].C(=O)([O-])[O-].[Na+].[Na+]>CO.O>[Cl:1][C:2]1[C:11]([CH:12]=[N:20][OH:19])=[C:10]([S:14]([CH3:17])(=[O:16])=[O:15])[CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 10340Sodium CarbonateHCID 21645Hydroxylamine HClHCID 18517410Methyl 2-chloro-3-formyl-4-methylsulfonylbenzoate

生成物 1

HCID 86584467Methyl 2-chloro-3-hydroxyiminomethyl-4-methylsulfonylbenzoate収率 96.6%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962
Water
溶媒
2 回

実験手順

55.23 g (0.199 mol) of methyl 2-chloro-3-formyl-4-methylsulfonylbenzoate are suspended in 400 ml of methanol/100 ml of water and treated with 15.27 g (0.219 mol) of hydroxylammonium chloride. 11.56 g (0.11 mol) of sodium carbonate—dissolved in 100 ml of water—are then slowly added dropwise at room temperature. After stirring at room temperature for 4 hours, the methanol is removed in a rotary evaporator, the residue is diluted with water and the mixture is extracted three times with dichlormethane. 56.05 g (96% of theory) of methyl 2-chloro-3 hydroximinomethyl-4-methylsulfonylbenzoate having a melting point of 126-130° C. are obtained.

後処理

  1. additionare then slowly added dropwise at room temperature
  2. customthe methanol is removed in a rotary evaporator
  3. additionthe residue is diluted with water
  4. extractionthe mixture is extracted three times with dichlormethane

出典と根拠

ORDレコード
ord-0d46fc7f029142a692be586fe3a9b785
出典データセット
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06211216B1

反応ノート

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