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Sulfuric Acid → HCID 58136859、化合物

HRID 657946
ノート
印刷プレビュー

反応式

HRID 657946 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

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

生成物 1

HCID 58136859HCID 58136859、化合物収率 164.6%

試薬・触媒・溶媒 3

HCID 17977687Phenyltrimethylammonium bromide dibromide
触媒
HCID 887Methanol溶媒
HCID 8028Tetrahydrofuran溶媒

反応条件

温度
60 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b6fe4e3db36a40eeaf365445e6a2dfa1
出典データセット
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08076336B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート