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

HRID 1276111
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HRID 1276111 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 10340Sodium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 18517410Methyl 2-chloro-3-formyl-4-methylsulfonylbenzoate

생성물 1

HCID 86584467Methyl 2-chloro-3-hydroxyiminomethyl-4-methylsulfonylbenzoate수율 91.4%

시약·촉매·용매 2

HCID 887Methanol용매
HCID 962
Water
용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-780dc9d11f9c4703be3790f505727c7c
출처 데이터셋
uspto-grants-2000_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06165944

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