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Sulfuric Acid → HCID 58136859, 화합물

HRID 532368
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HRID 532368 반응식
[C:1]([C:4]1[CH:5]=[C:6]([N:16]([CH3:23])[C:17](=[O:22])[C:18]([F:21])([F:20])[F:19])[CH:7]=[C:8]([S:10]([F:15])([F:14])([F:13])([F:12])[F:11])[CH:9]=1)(=[O:3])[CH3:2].[Br-:24].[Br-].[Br-].C1([N+](C)(C)C)C=CC=CC=1.C1([N+](C)(C)C)C=CC=CC=1.C1([N+](C)(C)C)C=CC=CC=1.S(=O)(=O)(O)O>CO.C1COCC1.[Br-].[Br-].[Br-].C1([N+](C)(C)C)C=CC=CC=1.C1([N+](C)(C)C)C=CC=CC=1.C1([N+](C)(C)C)C=CC=CC=1>[Br:24][CH2:2][C:1]([C:4]1[CH:5]=[C:6]([N:16]([CH3:23])[C:17](=[O:22])[C:18]([F:21])([F:19])[F:20])[CH:7]=[C:8]([S:10]([F:14])([F:15])([F:13])([F:12])[F:11])[CH:9]=1)=[O:3]
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7

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HCID 1118Sulfuric AcidHCID 17977687Phenyltrimethylammonium bromide dibromideHCID 58136869N-[3-Acetyl-5-(pentafluorosulfanyl)phenyl]-2,2,2-trifluoro-N-methylacetamide

생성물 1

HCID 58136859HCID 58136859, 화합물수율 164.6%

시약·촉매·용매 3

HCID 17977687Phenyltrimethylammonium bromide dibromide
촉매
HCID 887Methanol용매
HCID 8028Tetrahydrofuran용매

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온도
60 °C

실험 절차

N-[3-Acetyl-5-(pentafluorosulfanyl)phenyl]-2,2,2-trifluoro-N-methylacetamide (O2.075; 1.03 g) was dissolved in a mixture of methanol (20 ml) and THF (20 ml). Phenyltrimethylammonium tribromide (1.05 g) was added while stirring. After stirring at RT for 5 h, the mixture was left to stand overnight, then further phenyltrimethylammonium tribromide (100 mg) was added and the mixture was heated to 60° C. for 2 h. After cooling, the reaction mixture was added to 2 N sulfuric acid and stirred for 10 min. Then the aqueous phase was extracted three times with EA. The combined organic phases were dried over magnesium sulfate and, after the desiccant had been filtered off, dried under reduced pressure. 1.2 g of the title compound were obtained, which had sufficient purity for the next reactions.

후처리

  1. stirringAfter stirring at RT for 5 h
  2. waitthe mixture was left
  3. temperatureAfter cooling
  4. stirringstirred for 10 min
  5. extractionThen the aqueous phase was extracted three times with EA
  6. dry with materialThe combined organic phases were dried over magnesium sulfate
  7. filtrationafter the desiccant had been filtered off
  8. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-975a171d29054848bd474ab235e3c3a4
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08853206B2

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