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

HRID 1276111
ノート
印刷プレビュー

反応式

HRID 1276111 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.[NH2:19][OH:20].C(=O)([O-])[O-].[Na+].[Na+]>CO.O>[Cl:1][C:2]1[C:11]([CH:12]=[N:19][OH:20])=[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 443297Hydroxyamine hydrochlorideHCID 18517410Methyl 2-chloro-3-formyl-4-methylsulfonylbenzoate

生成物 1

HCID 86584467Methyl 2-chloro-3-hydroxyiminomethyl-4-methylsulfonylbenzoate収率 91.4%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒
HCID 962
Water
溶媒

実験手順

15.00 g (54 mmol) of methyl 2-chloro-3-formyl-4-methylsulfonylbenzoate and 4.20 g (60 mmol) of hydroxylamine hydrochloride were taken up in 300 ml of methanol, and a solution of 3.18 g (30 mmol) of sodium carbonate in 80 ml of water was added dropwise. After the mixture had been stirred at room temperature for 12 hours, the methanol was distilled off and the residue was diluted with water and extracted with diethyl ether. The organic phase was dried and the solvent was removed. 14.40 g (91% of theory) of methyl 2-chloro-3-hydroxyiminomethyl-4-methylsulfonylbenzoate were obtained.

後処理

  1. distillationthe methanol was distilled off
  2. additionthe residue was diluted with water
  3. extractionextracted with diethyl ether
  4. customThe organic phase was dried
  5. customthe solvent was removed

出典と根拠

ORDレコード
ord-780dc9d11f9c4703be3790f505727c7c
出典データセット
uspto-grants-2000_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06165944

反応ノート

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