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Sodium Hydroxide → 3-(N-ethyl-N-methylsulfamoylamino)-2,6-difluorobenzoic acid

HRID 2196740
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인쇄 미리보기

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HRID 2196740 반응식
[OH-].[Na+].[CH2:3]([N:5]([C:11]1[C:12]([F:22])=[C:13]([C:18]([F:21])=[CH:19][CH:20]=1)[C:14]([O:16]C)=[O:15])[S:6](=[O:10])(=[O:9])[NH:7][CH3:8])[CH3:4]>C1COCC1.CO>[CH2:3]([N:5]([C:11]1[C:12]([F:22])=[C:13]([C:18]([F:21])=[CH:19][CH:20]=1)[C:14]([OH:16])=[O:15])[S:6](=[O:9])(=[O:10])[NH:7][CH3:8])[CH3:4]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 67052525methyl 3-(N-ethyl-N-methylsulfamoylamino)-2,6-difluorobenzoate

생성물 1

HCID 670525023-(N-ethyl-N-methylsulfamoylamino)-2,6-difluorobenzoic acid수율 83.1%

시약·촉매·용매 1

HCID 21899815MeOH tetrahydrofuran용매

반응 조건

온도
60 °C

실험 절차

NaOH (0.908 mL, 1.82 mmol) was added to methyl 3-(N-ethyl-N-methylsulfamoylamino)-2,6-difluorobenzoate (0.280 g, 0.908 mmol) in THF-MeOH (3:2; 5 mL). The mixture was warmed to 60° C. for 16 hours. The cooled mixture was concentrated under reduced pressure, and the residue was taken up in 1M NaOH (4 mL) and washed with EtOAc. The aqueous pH was lowered to below 3 and extracted with EtOAc (3×6 mL) to provide crude 3-(N-ethyl-N-methylsulfamoylamino)-2,6-difluorobenzoic acid (222 mg, 83% yield).

후처리

  1. concentrationThe cooled mixture was concentrated under reduced pressure
  2. washwashed with EtOAc
  3. extractionextracted with EtOAc (3×6 mL)

출처 및 근거

ORD 기록
ord-550d36c9c4944d419e3698b0a9193050
출처 데이터셋
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08338452B2

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