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Acetic Anhydride → 3-Acetylamino-N-methoxy-N-methyl-5-(pentafluorosulfanyl)benzamide

HRID 217764
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HRID 217764 반응식
[NH2:1][C:2]1[CH:3]=[C:4]([CH:11]=[C:12]([S:14]([F:19])([F:18])([F:17])([F:16])[F:15])[CH:13]=1)[C:5]([N:7]([O:9][CH3:10])[CH3:8])=[O:6].C(N(CC)CC)C.[C:27](OC(=O)C)(=[O:29])[CH3:28].C(=O)([O-])O.[Na+]>C(Cl)Cl.O>[C:27]([NH:1][C:2]1[CH:3]=[C:4]([CH:11]=[C:12]([S:14]([F:19])([F:15])([F:16])([F:17])[F:18])[CH:13]=1)[C:5]([N:7]([O:9][CH3:10])[CH3:8])=[O:6])(=[O:29])[CH3:28]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 516892Sodium BicarbonateHCID 580857033-Amino-N-methoxy-N-methyl-5-pentafluorosulfanylbenzamide

생성물 1

HCID 581368203-Acetylamino-N-methoxy-N-methyl-5-(pentafluorosulfanyl)benzamide

시약·촉매·용매 2

HCID 962Water
용매
HCID 6344Dichloromethane용매

실험 절차

3-Amino-N-methoxy-N-methyl-5-pentafluorosulfanylbenzamide (1.2 g) was dissolved in methylene chloride (15 ml), and triethylamine (0.7 ml) followed by acetic anhydride (1.75 ml) were added while stirring with exclusion of moisture. After stirring at RT for 3 h, water and saturated sodium hydrogencarbonate solution were added, the phases were separated and the methylene chloride phase was washed three times more with water, dried over magnesium sulfate, filtered and concentrated. The resulting product (1.3 g) was used in the next stage without further purification.

후처리

  1. additionwere added
  2. stirringAfter stirring at RT for 3 h
  3. customthe phases were separated
  4. washthe methylene chloride phase was washed three times more with water
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe resulting product (1.3 g) was used in the next stage without further purification

출처 및 근거

ORD 기록
ord-03950caeda10463a81f557a277401664
출처 데이터셋
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08198272B2

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