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Water → 2-Chloro-N-methoxy-N-methylbenzamide

HRID 1027684
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HRID 1027684 반응식
[Cl:1][C:2]1[CH:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4](Cl)=[O:5].Cl.[CH3:12][NH:13][O:14][CH3:15].N1C=CC=CC=1.O>ClCCl>[Cl:1][C:2]1[CH:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([N:13]([O:14][CH3:15])[CH3:12])=[O:5]
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참가 물질

6

반응물 4

HCID 962WaterHCID 1049PyridineHCID 691102-Chlorobenzoyl chlorideHCID 81138Methanamine, N-methoxy-, hydrochloride (1:1)

생성물 1

HCID 181853702-Chloro-N-methoxy-N-methylbenzamide수율 85.2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 2-chlorobenzoyl chloride (8 g, 46 mmol) in dichloromethane (200 mL) at 0° C. was added N,O-dimethylhydroxylamine hydrochloride (4.9 g, 50 mmol) followed by pyridine (11 mL, 137 mmol). The mixture was stirred at room temperature for 16 hours. Water was added to the reaction mixture and organic layer was washed with brine, dried over magnesium sulfate and concentrated. Purification by chromatography on silica gel gave 2-chloro-N-methoxy-N-methylbenzamide (21) (7.8 g, 39.2 mmol, 85%) as clear oil.

후처리

  1. washwas washed with brine
  2. dry with materialdried over magnesium sulfate
  3. concentrationconcentrated
  4. customPurification by chromatography on silica gel

출처 및 근거

ORD 기록
ord-b72fea5e90fd4ee0b7a6e5bfe9b98fa0
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08735399B2

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