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Water → 1-Methanesulfonyloxy-6,6,7,7,7-pentafluoroheptane

HRID 1267741
ノート
印刷プレビュー

反応式

HRID 1267741 の反応式
C(N(CC)CC)C.[CH3:8][S:9](Cl)(=[O:11])=[O:10].[F:13][C:14]([F:25])([C:21]([F:24])([F:23])[F:22])[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][OH:20].O>ClCCl>[CH3:8][S:9]([O:20][CH2:19][CH2:18][CH2:17][CH2:16][CH2:15][C:14]([F:25])([F:13])[C:21]([F:22])([F:23])[F:24])(=[O:11])=[O:10]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 120170636,6,7,7,7-Pentafluoroheptan-1-ol

生成物 1

HCID 120170641-Methanesulfonyloxy-6,6,7,7,7-pentafluoroheptane収率 82.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Triethylamine (25.83 ml, 185.3 mmol) and methanesulfonyl chloride (6.9 ml, 88.9 mmol) were added dropwise to a solution of 6,6,7,7,7-pentafluoroheptan-1-ol (14.1 g, 74.1 mmol) in dichloromethane (350 ml) at 0° C., followed by stirring for 1 hour. After the reaction was completed, water was added to the reaction mixture, which was then extracted twice with dichloromethane. The combined organic layers were washed with water and saturated aqueous sodium chloride, and then dried over anhydrous magnesium sulfate. After distilling off the solvent, the residue was purified by silica gel column chromatography (eluent: ethyl acetate/hexane=1/10) to give 1-methanesulfonyloxy-6,6,7,7,7-pentafluoroheptane (17.3 g, Yield 82%).

後処理

  1. extractionwas then extracted twice with dichloromethane
  2. washThe combined organic layers were washed with water and saturated aqueous sodium chloride
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationAfter distilling off the solvent
  5. customthe residue was purified by silica gel column chromatography (eluent: ethyl acetate/hexane=1/10)

出典と根拠

ORDレコード
ord-cdd26ddf1c6246c7864ac58b959853a6
出典データセット
uspto-grants-2003_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06552068B1

反応ノート

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